#------------------------------------------------------------------------------ #$Date: 2026-03-26 01:51:31 +0000 (Thu, 26 Mar 2026) $ #$Revision: 305181 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/43/7064347.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7064347 loop_ _publ_author_name 'Rayasingh, Amlan Ranjan' 'Manivannan, Vadivelu' _publ_section_title ; Synthesis, Structure, Catalytic, and Bio Activity of Some Metal Complexes and Coordination Polymer Featuring Imidazo[1,5-a]pyridine and Chromen[4,3-b]pyrrole-4-one ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D6NJ00431H _journal_year 2026 _chemical_formula_moiety 'C36 H29.322 Br2 N6 Ni O3, 2(Cl), 0.5[CH4O]' _chemical_formula_sum 'C36 H30 Br2 Cl2 N6 Ni O3' _chemical_formula_weight 884.09 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2025-04-21 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2025-05-24 deposited with the CCDC. 2026-03-24 downloaded from the CCDC. ; _cell_angle_alpha 94.067(5) _cell_angle_beta 109.340(4) _cell_angle_gamma 102.568(4) _cell_formula_units_Z 2 _cell_length_a 11.2189(17) _cell_length_b 12.5312(19) _cell_length_c 14.612(2) _cell_measurement_reflns_used 8650 _cell_measurement_temperature 295.00 _cell_measurement_theta_max 24.220 _cell_measurement_theta_min 2.255 _cell_volume 1868.9(5) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 295.00 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.960 _diffrn_measured_fraction_theta_max 0.961 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_unetI/netI 0.0692 _diffrn_reflns_Laue_measured_fraction_full 0.960 _diffrn_reflns_Laue_measured_fraction_max 0.961 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 35819 _diffrn_reflns_point_group_measured_fraction_full 0.960 _diffrn_reflns_point_group_measured_fraction_max 0.961 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.696 _diffrn_reflns_theta_min 2.019 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_target Mo _diffrn_source_type 'Incoatec I\ms' _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 2.844 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.5203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0916 before and 0.0606 after correction. The Ratio of minimum to maximum transmission is 0.6981. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.571 _exptl_crystal_description block _exptl_crystal_F_000 888 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.190 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.117 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 448 _refine_ls_number_reflns 6849 _refine_ls_number_restraints 1244 _refine_ls_restrained_S_all 1.010 _refine_ls_R_factor_all 0.1932 _refine_ls_R_factor_gt 0.0999 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2690 _refine_ls_wR_factor_ref 0.3506 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2972 _reflns_number_total 6849 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 107_2ni_0m_a_a.res in P-1 107_2ni_0m_a.res created by SHELXL-2018/3 at 23:13:42 on 21-Apr-2025 REM Old TITL 107_2ni_0m_a_a.res in P-1 REM SHELXT solution in P-1: R1 0.245, Rweak 0.018, Alpha 0.077 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: Br3 C39 N4 Ni2 O7 CELL 0.71073 11.2189 12.5312 14.6124 94.067 109.34 102.568 ZERR 2 0.0017 0.0019 0.0023 0.005 0.004 0.004 LATT 1 SFAC C H Br Cl N Ni O UNIT 72 60 4 4 12 2 6 SADI Br1 C36 Br4 C2A RIGU SIMU DFIX 0.85 O2 H2a O2 H2b DFIX 0.85 O3 H3a O3 H3b SADI C30 C31 C30 C38 DANG 1.34 H2a H2b SADI Ni1 H2a Ni1 H2b DANG 1.34 H3a H3b SADI C31 C32 C38 C0 SADI C31 C36 C38 C2A SADI C32 C33 C0 C39 SADI C34 C33 C40 C39 SADI C34 C35 C40 C37 SADI C35 C36 C37 C2A SADI 0.04 Br1 C31 Br4 C38 SADI 0.04 Br1 C35 Br4 C37 SADI 0.04 C30 C32 C30 C0 SADI 0.04 C30 C36 C30 C2A SADI 0.04 C31 C33 C38 C39 SADI 0.04 C31 C35 C38 C37 SADI 0.04 C32 C34 C0 C40 SADI 0.04 C32 C36 C0 C2A SADI 0.04 C34 C36 C40 C2A SADI 0.04 C33 C35 C39 C37 SADI 0.1 C31 C32 C36 C35 C33 C34 DFIX 1.4 C33 C34 FLAT C34 C33 C32 C31 C36 C35 SADI 0.1 C37 C38 C2A C0 C40 C39 EADP C31 C32 C34 C33 C35 C36 Br4 C2A C37 C38 C0 C39 C40 Br1 EADP Cl2 Cl3 DFIX 1.4 C17 C16 SADI Ni1 H1a Ni1 H1b SADI Br2 C14 Br2A C14A SADI C13 C18 C13 C18A SADI C13 C14 C13 C14A SADI C18 C17 C18A C17A SADI C14 C15 C14A C15A SADI C15 C16 C15A C16A SADI C16 C17 C16A C17A SADI 0.04 Br2 C13 Br2A C13 SADI 0.04 Br2 C15 Br2A C15A SADI 0.04 C13 C15 C13 C15A SADI 0.04 C13 C17 C13 C17A SADI 0.04 C18 C16 C18A C16A SADI 0.04 C14 C16 C14A C16A SADI 0.04 C15 C17 C15A C17A DFIX 2.5 Br2A O3 EADP Br2A C13 C18 C15 C16 C17 C14A C15A C16A C17A Br2 C14 C18A DELU C13 C18 C15 C16 C17 C14A C15A C16A C17A Br2A C14 C18A Br2 L.S. 10 PLAN 6 SIZE 0.12 0.08 0.04 TEMP 21.85 CONF list 4 MORE -1 BOND $H fmap 2 acta OMIT -10 6 3 OMIT -10 9 11 OMIT -10 10 3 OMIT -9 -4 6 OMIT -9 -2 7 OMIT -9 -1 10 OMIT -9 7 2 OMIT -9 7 6 OMIT -9 7 10 OMIT -9 8 6 OMIT -8 -6 4 OMIT -8 -5 4 OMIT -8 0 8 OMIT -7 -4 8 OMIT -7 -4 11 OMIT -7 -3 7 OMIT -7 -3 9 OMIT -7 -2 8 OMIT -7 -1 3 OMIT -7 0 4 OMIT -7 2 4 OMIT -7 4 1 OMIT -7 4 3 OMIT -7 6 7 OMIT -7 8 5 OMIT -7 8 7 OMIT -7 9 5 OMIT -6 -7 1 OMIT -6 -5 6 OMIT -6 -4 11 OMIT -6 -3 5 OMIT -6 -1 4 OMIT -6 -1 5 OMIT -6 0 5 OMIT -6 2 13 OMIT -6 12 1 OMIT -5 -8 4 OMIT -5 -7 5 OMIT -5 -5 8 OMIT -5 -4 5 OMIT -5 -3 6 OMIT -5 -3 8 OMIT -5 -1 3 OMIT -5 0 3 OMIT -5 2 1 OMIT -5 2 9 OMIT -5 3 1 OMIT -5 3 4 OMIT -5 4 1 OMIT -5 5 2 OMIT -5 6 1 OMIT -5 7 1 OMIT -5 7 4 OMIT -5 8 2 OMIT -5 8 3 OMIT -5 9 2 OMIT -5 10 3 OMIT -4 -6 1 OMIT -4 -3 2 OMIT -4 -2 6 OMIT -4 -1 2 OMIT -4 2 4 OMIT -4 5 1 OMIT -4 5 3 OMIT -4 5 6 OMIT -4 9 2 OMIT -4 10 2 OMIT -3 -9 2 OMIT -3 -6 9 OMIT -3 -6 10 OMIT -3 -5 6 OMIT -3 -3 8 OMIT -3 -2 1 OMIT -3 -2 3 OMIT -3 -2 8 OMIT -3 -1 9 OMIT -3 -1 14 OMIT -3 1 0 OMIT -3 3 1 OMIT -3 4 0 OMIT -3 4 4 OMIT -3 5 8 OMIT -3 6 1 OMIT -3 6 3 OMIT -3 7 1 OMIT -3 9 1 OMIT -3 10 2 OMIT -2 -7 2 OMIT -2 -6 1 OMIT -2 -6 3 OMIT -2 -6 4 OMIT -2 -6 5 OMIT -2 -5 1 OMIT -2 -5 3 OMIT -2 -5 4 OMIT -2 -4 4 OMIT -2 -1 3 OMIT -2 -1 6 OMIT -2 -1 7 OMIT -2 -1 8 OMIT -2 0 2 OMIT -2 0 4 OMIT -2 0 5 OMIT -2 1 1 OMIT -2 1 5 OMIT -2 3 4 OMIT -2 4 0 OMIT -2 4 1 OMIT -2 5 0 OMIT -2 5 1 OMIT -2 6 0 OMIT -2 6 1 OMIT -2 8 2 OMIT -2 8 5 OMIT -2 9 4 OMIT -2 9 5 OMIT -1 -7 2 OMIT -1 -6 3 OMIT -1 -6 8 OMIT -1 -4 2 OMIT -1 -4 4 OMIT -1 -4 8 OMIT -1 -4 9 OMIT -1 -3 2 OMIT -1 -3 3 OMIT -1 -3 11 OMIT -1 -2 1 OMIT -1 -2 2 OMIT -1 -2 10 OMIT -1 -1 2 OMIT -1 -1 7 OMIT -1 0 2 OMIT -1 0 5 OMIT -1 0 8 OMIT -1 0 10 OMIT -1 1 1 OMIT -1 1 6 OMIT -1 1 9 OMIT -1 2 1 OMIT -1 2 3 OMIT -1 2 4 OMIT -1 3 4 OMIT -1 4 3 OMIT -1 5 0 OMIT -1 7 5 OMIT -1 9 3 OMIT 0 -10 4 OMIT 0 -7 2 OMIT 0 -7 4 OMIT 0 -6 4 OMIT 0 -5 5 OMIT 0 -4 1 OMIT 0 -4 9 OMIT 0 -4 12 OMIT 0 -3 1 OMIT 0 -3 5 OMIT 0 -3 12 OMIT 0 -2 1 OMIT 0 -2 2 OMIT 0 -1 3 OMIT 0 0 1 OMIT 0 0 11 OMIT 0 1 11 OMIT 0 2 0 OMIT 0 2 1 OMIT 0 2 3 OMIT 0 2 11 OMIT 0 3 1 OMIT 0 3 4 OMIT 0 4 1 OMIT 0 4 2 OMIT 0 4 3 OMIT 0 6 0 OMIT 0 6 9 OMIT 0 8 7 OMIT 1 -13 4 OMIT 1 -9 2 OMIT 1 -8 3 OMIT 1 -8 8 OMIT 1 -7 1 OMIT 1 -6 4 OMIT 1 -6 6 OMIT 1 -5 1 OMIT 1 -5 9 OMIT 1 -4 1 OMIT 1 -4 6 OMIT 1 -4 9 OMIT 1 -3 9 OMIT 1 -2 1 OMIT 1 -2 3 OMIT 1 -2 6 OMIT 1 -1 1 OMIT 1 -1 2 OMIT 1 0 0 OMIT 1 0 1 OMIT 1 0 2 OMIT 1 0 10 OMIT 1 1 0 OMIT 1 1 2 OMIT 1 3 6 OMIT 1 4 0 OMIT 1 6 2 OMIT 2 -9 4 OMIT 2 -8 7 OMIT 2 -7 3 OMIT 2 -7 7 OMIT 2 -6 3 OMIT 2 -6 4 OMIT 2 -6 6 OMIT 2 -5 6 OMIT 2 -5 11 OMIT 2 -4 10 OMIT 2 -3 1 OMIT 2 -3 4 OMIT 2 -3 8 OMIT 2 -2 2 OMIT 2 -2 9 OMIT 2 -1 2 OMIT 2 0 0 OMIT 2 0 6 OMIT 2 2 0 OMIT 2 4 2 OMIT 3 -11 1 OMIT 3 -10 2 OMIT 3 -7 1 OMIT 3 -6 1 OMIT 3 -6 6 OMIT 3 -5 2 OMIT 3 -5 4 OMIT 3 -4 3 OMIT 3 -4 4 OMIT 3 -4 9 OMIT 3 -3 1 OMIT 3 -2 2 OMIT 3 -1 8 OMIT 3 0 2 OMIT 3 2 4 OMIT 3 2 11 OMIT 3 4 0 OMIT 3 4 5 OMIT 3 5 0 OMIT 4 -12 3 OMIT 4 -9 1 OMIT 4 -9 2 OMIT 4 -8 5 OMIT 4 -8 10 OMIT 4 -6 3 OMIT 4 -5 2 OMIT 4 -4 2 OMIT 4 -4 6 OMIT 4 -3 4 OMIT 4 2 1 OMIT 5 -9 1 OMIT 5 -8 1 OMIT 5 -5 6 OMIT 5 -2 4 OMIT 5 1 1 OMIT 5 3 2 OMIT 6 -5 7 OMIT 6 -4 2 OMIT 6 -1 1 OMIT 6 1 0 OMIT 7 1 6 OMIT 7 3 0 OMIT 8 1 3 OMIT 9 -1 1 REM REM REM WGHT 0.200000 FVAR 0.35462 0.68657 0.65479 0.76085 NI1 6 0.211441 0.787079 0.701958 11.00000 0.06366 0.08158 = 0.07286 0.00794 0.02528 0.01898 PART 1 BR1 3 0.598324 0.617004 0.870644 21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 BR2 3 0.310022 0.459104 0.889596 41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 CL1 4 0.283772 0.790471 0.407478 31.00000 0.13920 0.17272 = 0.12825 0.03801 0.06902 0.02792 PART 0 N1 5 0.043113 0.659652 0.663827 11.00000 0.06408 0.10441 = 0.06166 0.02052 0.02125 0.01934 N5 5 0.300322 0.772256 0.848706 11.00000 0.06348 0.07841 = 0.07419 -0.00197 0.01916 0.02269 N2 5 0.276730 0.651875 0.661442 11.00000 0.07059 0.07175 = 0.07263 -0.00763 0.03013 0.00600 O2 7 0.120434 0.901143 0.744060 11.00000 0.10424 0.11560 = 0.09026 0.02420 0.03747 0.05352 H2A 2 0.189842 0.943009 0.786222 11.00000 -1.50000 H2B 2 0.112374 0.933485 0.693107 11.00000 -1.50000 AFIX 6 O1 7 0.138943 0.817943 0.555149 11.00000 0.10434 0.13318 = 0.08218 0.03529 0.03978 0.02847 H1A 2 0.207079 0.849746 0.544547 11.00000 -1.50000 H1B 2 0.100794 0.868813 0.558942 11.00000 -1.50000 AFIX 0 N4 5 0.381375 0.913426 0.740697 11.00000 0.08878 0.07341 = 0.09490 0.00808 0.04450 0.02703 N3 5 0.366777 0.518475 0.639892 11.00000 0.08747 0.08818 = 0.08043 -0.00973 0.03869 0.02137 N6 5 0.390281 0.729272 0.993770 11.00000 0.09720 0.08088 = 0.06577 -0.00209 0.01956 0.03923 C23 1 0.053207 0.555011 0.637286 11.00000 0.06400 0.09978 = 0.05118 0.00542 0.01616 0.00644 C24 1 0.186116 0.553139 0.642072 11.00000 0.06389 0.08001 = 0.05551 0.00222 0.02175 0.00006 C25 1 0.234104 0.467213 0.626599 11.00000 0.08503 0.08536 = 0.06027 0.00145 0.02531 0.01417 C30 1 0.388156 0.629648 0.660125 11.00000 0.08118 0.09180 = 0.08784 -0.01456 0.03282 0.02992 C6 1 0.424232 0.841458 0.890134 11.00000 0.06955 0.06997 = 0.08660 -0.00842 0.01859 0.02055 CL3 4 0.030546 1.036098 0.582599 10.50000 0.30230 0.18081 = 0.39426 0.11582 0.16741 0.13004 C12 1 0.283025 0.703752 0.913287 11.00000 0.08285 0.08136 = 0.06702 -0.00198 0.01944 0.03688 C22 1 -0.054702 0.463770 0.611723 11.00000 0.07319 0.11719 = 0.06920 0.00423 0.01315 -0.01150 AFIX 43 H22 2 -0.048214 0.392349 0.596829 11.00000 -1.20000 AFIX 0 C5 1 0.468244 0.921817 0.832252 11.00000 0.06867 0.06237 = 0.10905 -0.00407 0.03382 0.02066 C13 1 0.168053 0.610314 0.898587 11.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 PART 1 C31 1 0.520041 0.704940 0.693950 21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 PART 0 C7 1 0.484622 0.817193 0.981875 11.00000 0.07336 0.07913 = 0.08879 -0.00734 0.00976 0.03197 C26 1 0.197395 0.348970 0.605357 11.00000 0.09959 0.08457 = 0.06182 0.00291 0.00505 0.01101 AFIX 43 H26 2 0.113260 0.311088 0.598905 11.00000 -1.20000 AFIX 0 C4 1 0.585673 0.999884 0.869339 11.00000 0.07327 0.07797 = 0.14006 -0.00498 0.03301 0.02078 AFIX 43 H4 2 0.644414 1.005062 0.932722 11.00000 -1.20000 AFIX 0 C11 1 0.412941 0.681170 1.076513 11.00000 0.13470 0.10312 = 0.06420 0.00647 0.00787 0.04770 AFIX 43 H11 2 0.350017 0.623261 1.082984 11.00000 -1.20000 AFIX 0 C19 1 -0.074833 0.669627 0.658450 11.00000 0.06156 0.14581 = 0.09448 0.01033 0.02496 0.02588 AFIX 43 H19 2 -0.083194 0.739880 0.675293 11.00000 -1.20000 AFIX 0 C27 1 0.280436 0.291065 0.594462 11.00000 0.12329 0.09274 = 0.08697 -0.00463 0.02852 0.01674 AFIX 43 H27 2 0.254072 0.214187 0.580940 11.00000 -1.20000 AFIX 0 C1 1 0.409411 0.985594 0.681021 11.00000 0.11285 0.08787 = 0.14515 0.03381 0.07303 0.03883 AFIX 43 H1 2 0.350496 0.981078 0.617823 11.00000 -1.20000 AFIX 0 C28 1 0.414128 0.350255 0.604088 11.00000 0.12943 0.09888 = 0.10952 -0.01421 0.05182 0.02973 AFIX 43 H28 2 0.471025 0.310668 0.594013 11.00000 -1.20000 AFIX 0 C8 1 0.605522 0.857906 1.057025 11.00000 0.07900 0.09844 = 0.11254 -0.00824 0.00306 0.03137 AFIX 43 H8 2 0.669228 0.915875 1.051565 11.00000 -1.20000 AFIX 0 C3 1 0.611056 1.072838 0.803130 11.00000 0.09440 0.07838 = 0.17490 0.00100 0.06511 0.01288 AFIX 43 H3 2 0.690196 1.126451 0.823797 11.00000 -1.20000 AFIX 0 PART 1 C32 1 0.542893 0.779374 0.625879 21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 AFIX 43 H32 2 0.478464 0.774875 0.565073 21.00000 -1.20000 AFIX 0 PART 0 C21 1 -0.176118 0.485294 0.609492 11.00000 0.07241 0.15304 = 0.10100 0.01259 0.02546 -0.00979 AFIX 43 H21 2 -0.250513 0.426976 0.592928 11.00000 -1.20000 AFIX 0 C29 1 0.453499 0.459879 0.627093 11.00000 0.10293 0.10174 = 0.11284 -0.01336 0.04991 0.03363 AFIX 43 H29 2 0.538290 0.497034 0.634557 11.00000 -1.20000 AFIX 0 C20 1 -0.182435 0.584872 0.630300 11.00000 0.07360 0.16512 = 0.09383 0.01347 0.02580 0.01188 AFIX 43 H20 2 -0.262323 0.598375 0.625820 11.00000 -1.20000 AFIX 0 PART 1 C18 1 0.044366 0.648154 0.898986 41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 AFIX 43 H18 2 0.045592 0.721949 0.913469 41.00000 -1.20000 AFIX 0 C14 1 0.159329 0.505865 0.887579 41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 PART 0 C2 1 0.528804 1.067197 0.716232 11.00000 0.12378 0.09218 = 0.16187 0.02247 0.07391 0.01957 AFIX 43 H2 2 0.548431 1.117558 0.676260 11.00000 -1.20000 AFIX 0 C10 1 0.532905 0.721948 1.150075 11.00000 0.13554 0.11518 = 0.09272 0.01305 0.00209 0.05843 AFIX 43 H10 2 0.551804 0.691197 1.207661 11.00000 -1.20000 AFIX 0 C9 1 0.625833 0.808049 1.139606 11.00000 0.12388 0.09708 = 0.10264 -0.01884 -0.01097 0.03523 AFIX 43 H9 2 0.705826 0.833351 1.190921 11.00000 -1.20000 AFIX 0 PART 1 C15 1 0.037975 0.417741 0.871986 41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 AFIX 43 H15 2 0.034857 0.342726 0.865174 41.00000 -1.20000 AFIX 0 C34 1 0.753178 0.852883 0.748339 21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 AFIX 43 H34 2 0.834087 0.903902 0.767446 21.00000 -1.20000 AFIX 0 C33 1 0.662164 0.857015 0.653143 21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 AFIX 43 H33 2 0.681755 0.907539 0.613286 21.00000 -1.20000 AFIX 0 C16 1 -0.060858 0.453666 0.868777 41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 AFIX 43 H16 2 -0.136917 0.400216 0.860841 41.00000 -1.20000 AFIX 0 C35 1 0.738320 0.788759 0.810427 21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 AFIX 43 H35 2 0.802357 0.794425 0.871666 21.00000 -1.20000 AFIX 0 C17 1 -0.069218 0.560964 0.875534 41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 AFIX 43 H17 2 -0.149770 0.576421 0.864668 41.00000 -1.20000 AFIX 0 PART 0 CL2 4 0.004434 1.129256 0.913467 10.50000 0.30230 0.18081 = 0.39426 0.11582 0.16741 0.13004 PART 1 C36 1 0.618354 0.709709 0.778835 21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 PART 2 BR4 3 0.617097 0.646284 0.836860 -21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 C2A 1 0.609333 0.737892 0.742728 -21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 C37 1 0.727758 0.803490 0.750764 -21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 AFIX 43 H37 2 0.805459 0.802235 0.799600 -21.00000 -1.20000 AFIX 0 C38 1 0.502498 0.713479 0.661355 -21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 C0 1 0.494011 0.785930 0.587567 -21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 AFIX 43 H0 2 0.415397 0.781900 0.537401 -21.00000 -1.20000 AFIX 0 C39 1 0.609442 0.861940 0.595479 -21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 AFIX 43 H39 2 0.615187 0.906427 0.548010 -21.00000 -1.20000 AFIX 0 C40 1 0.722900 0.866092 0.686221 -21.00000 0.09133 0.13036 = 0.10917 0.00347 0.02818 0.04499 AFIX 43 H40 2 0.798681 0.920983 0.696473 -21.00000 -1.20000 AFIX 0 CL 4 0.189704 0.832373 0.375957 -31.00000 0.15472 0.13623 = 0.15675 0.03876 0.09367 0.02216 PART 0 O3 7 0.107520 0.941863 0.943822 11.00000 0.08407 0.18327 = 0.11161 -0.08528 0.01701 0.00927 H3A 2 0.126145 0.915779 0.896440 11.00000 -1.50000 H3B 2 0.084499 1.000127 0.923863 11.00000 -1.50000 PART 2 C18A 1 0.192401 0.491923 0.879377 -41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 AFIX 43 H18A 2 0.272459 0.482533 0.879570 -41.00000 -1.20000 AFIX 0 C14A 1 0.052093 0.610892 0.887814 -41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 C15A 1 -0.058182 0.513435 0.875730 -41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 AFIX 43 H15A 2 -0.138192 0.519399 0.878408 -41.00000 -1.20000 AFIX 0 C16A 1 -0.031972 0.421164 0.861370 -41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 AFIX 43 H16A 2 -0.100355 0.358367 0.848780 -41.00000 -1.20000 AFIX 0 C17A 1 0.083859 0.402902 0.862144 -41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 AFIX 43 H17A 2 0.090693 0.330838 0.851148 -41.00000 -1.20000 AFIX 0 BR2A 3 0.052524 0.752208 0.942684 -41.00000 0.11797 0.10738 = 0.11467 -0.00285 0.03372 0.05180 HKLF 4 REM 107_2ni_0m_a_a.res in P-1 REM wR2 = 0.3506, GooF = S = 1.066, Restrained GooF = 1.010 for all data REM R1 = 0.0999 for 2972 Fo > 4sig(Fo) and 0.1932 for all 6849 data REM 448 parameters refined using 1244 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.190, deepest hole -0.748, 1-sigma level 0.117 Q1 1 0.0561 0.8545 0.2560 11.00000 0.05 1.19 Q2 1 0.4225 0.7986 0.5188 11.00000 0.05 1.09 Q3 1 0.0902 1.0829 0.6611 11.00000 0.05 0.76 Q4 1 0.0464 0.6972 0.9191 11.00000 0.05 0.75 Q5 1 0.1017 0.9000 0.9520 11.00000 0.05 0.66 Q6 1 0.3439 0.4756 0.8785 11.00000 0.05 0.65 REM The information below was added by Olex2. REM REM R1 = 0.0999 for 2972 Fo > 4sig(Fo) and 0.1932 for all 38138 data REM 448 parameters refined using n/a restraints REM Highest difference peak 1.19, deepest hole -0.75 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1932 REM R1_gt = 0.0999 REM wR_ref = 0.3506 REM GOOF = 1.066 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 38138 REM Reflections_gt = 2972 REM Parameters = 448 REM Hole = -0.75 REM Peak = 1.19 REM Flack = n/a ; _cod_data_source_file d6nj00431h2.cif _cod_data_source_block 1g _cod_original_cell_volume 1869.0(5) _cod_database_code 7064347 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.895 _shelx_estimated_absorpt_t_min 0.727 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2. Restrained distances O2-H2A = O2-H2B 0.85 with sigma of 0.02 O3-H3A = O3-H3B 0.85 with sigma of 0.02 C33-C34 1.4 with sigma of 0.02 C17-C16 1.4 with sigma of 0.02 Br2A-O3 2.5 with sigma of 0.02 H2A-H2B 1.34 with sigma of 0.04 H3A-H3B 1.34 with sigma of 0.04 Br1-C36 \\sim Br4-C2A with sigma of 0.02 C30-C31 \\sim C30-C38 with sigma of 0.02 Ni1-H2A \\sim Ni1-H2B with sigma of 0.02 C31-C32 \\sim C38-C0 with sigma of 0.02 C31-C36 \\sim C38-C2A with sigma of 0.02 C32-C33 \\sim C0-C39 with sigma of 0.02 C34-C33 \\sim C40-C39 with sigma of 0.02 C34-C35 \\sim C40-C37 with sigma of 0.02 C35-C36 \\sim C37-C2A with sigma of 0.02 Br1-C31 \\sim Br4-C38 with sigma of 0.04 Br1-C35 \\sim Br4-C37 with sigma of 0.04 C30-C32 \\sim C30-C0 with sigma of 0.04 C30-C36 \\sim C30-C2A with sigma of 0.04 C31-C33 \\sim C38-C39 with sigma of 0.04 C31-C35 \\sim C38-C37 with sigma of 0.04 C32-C34 \\sim C0-C40 with sigma of 0.04 C32-C36 \\sim C0-C2A with sigma of 0.04 C34-C36 \\sim C40-C2A with sigma of 0.04 C33-C35 \\sim C39-C37 with sigma of 0.04 C31-C32 \\sim C36-C35 \\sim C33-C34 with sigma of 0.1 C37-C38 \\sim C2A-C0 \\sim C40-C39 with sigma of 0.1 Ni1-H1A \\sim Ni1-H1B with sigma of 0.02 Br2-C14 \\sim Br2A-C14A with sigma of 0.02 C13-C18 \\sim C13-C18A with sigma of 0.02 C13-C14 \\sim C13-C14A with sigma of 0.02 C18-C17 \\sim C18A-C17A with sigma of 0.02 C14-C15 \\sim C14A-C15A with sigma of 0.02 C15-C16 \\sim C15A-C16A with sigma of 0.02 C16-C17 \\sim C16A-C17A with sigma of 0.02 Br2-C13 \\sim Br2A-C13 with sigma of 0.04 Br2-C15 \\sim Br2A-C15A with sigma of 0.04 C13-C15 \\sim C13-C15A with sigma of 0.04 C13-C17 \\sim C13-C17A with sigma of 0.04 C18-C16 \\sim C18A-C16A with sigma of 0.04 C14-C16 \\sim C14A-C16A with sigma of 0.04 C15-C17 \\sim C15A-C17A with sigma of 0.04 3. Restrained planarity C34, C33, C32, C31, C36, C35 with sigma of 0.1 4. Rigid bond restraints C13, C18, C15, C16, C17, C14A, C15A, C16A, C17A, Br2A, C14, C18A, Br2 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uanis(C31) = Uanis(C32) = Uanis(C34) = Uanis(C33) = Uanis(C35) = Uanis(C36) = Uanis(Br4) = Uanis(C2A) = Uanis(C37) = Uanis(C38) = Uanis(C0) = Uanis(C39) = Uanis(C40) = Uanis(Br1) Uanis(Cl2) = Uanis(Cl3) Uanis(Br2A) = Uanis(C13) = Uanis(C18) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C14A) = Uanis(C15A) = Uanis(C16A) = Uanis(C17A) = Uanis(Br2) = Uanis(C14) = Uanis(C18A) 6. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 7. Others Sof(Br4)=Sof(C2A)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(C0)=Sof(H0)=Sof(C39)= Sof(H39)=Sof(C40)=Sof(H40)=1-FVAR(1) Sof(Br1)=Sof(C31)=Sof(C32)=Sof(H32)=Sof(C34)=Sof(H34)=Sof(C33)=Sof(H33)= Sof(C35)=Sof(H35)=Sof(C36)=FVAR(1) Sof(Cl)=1-FVAR(2) Sof(Cl1)=FVAR(2) Sof(C18A)=Sof(H18A)=Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)= Sof(C17A)=Sof(H17A)=Sof(Br2A)=1-FVAR(3) Sof(Br2)=Sof(C18)=Sof(H18)=Sof(C14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)= Sof(C17)=Sof(H17)=FVAR(3) Fixed Sof: Cl3(0.5) Cl2(0.5) 8.a Free rotating group: O1(H1A,H1B) 8.b Aromatic/amide H refined with riding coordinates: C22(H22), C26(H26), C4(H4), C11(H11), C19(H19), C27(H27), C1(H1), C28(H28), C8(H8), C3(H3), C32(H32), C21(H21), C29(H29), C20(H20), C18(H18), C2(H2), C10(H10), C9(H9), C15(H15), C34(H34), C33(H33), C16(H16), C35(H35), C17(H17), C37(H37), C0(H0), C39(H39), C40(H40), C18A(H18A), C15A(H15A), C16A(H16A), C17A(H17A) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.21144(10) 0.78708(9) 0.70196(8) 0.0726(5) Uani 1 1 d D . . . . Br1 Br 0.5983(3) 0.6170(3) 0.8706(3) 0.1103(10) Uani 0.687(8) 1 d D U P A 1 Br2 Br 0.31002(17) 0.45910(14) 0.88960(12) 0.1126(6) Uani 0.761(2) 1 d D U P B 1 Cl1 Cl 0.2838(9) 0.7905(7) 0.4075(5) 0.142(4) Uani 0.655(17) 1 d . U P C 1 N1 N 0.0431(7) 0.6597(7) 0.6638(5) 0.0770(18) Uani 1 1 d . U . . . N5 N 0.3003(7) 0.7723(6) 0.8487(5) 0.0734(17) Uani 1 1 d . U . . . N2 N 0.2767(7) 0.6519(6) 0.6614(5) 0.0735(17) Uani 1 1 d . U . . . O2 O 0.1204(7) 0.9011(6) 0.7441(5) 0.098(2) Uani 1 1 d D . . . . H2A H 0.190(6) 0.943(7) 0.786(6) 0.147 Uiso 1 1 d D U . . . H2B H 0.112(11) 0.933(7) 0.693(4) 0.147 Uiso 1 1 d D U . . . O1 O 0.1389(8) 0.8179(7) 0.5551(6) 0.104(2) Uani 1 1 d G . . . . H1A H 0.207079 0.849746 0.544547 0.156 Uiso 1 1 d DG U . . . H1B H 0.100794 0.868813 0.558942 0.156 Uiso 1 1 d DG U . . . N4 N 0.3814(8) 0.9134(6) 0.7407(6) 0.0819(19) Uani 1 1 d . U . . . N3 N 0.3668(8) 0.5185(7) 0.6399(6) 0.084(2) Uani 1 1 d . U . . . N6 N 0.3903(8) 0.7293(6) 0.9938(5) 0.0817(18) Uani 1 1 d . U . . . C23 C 0.0532(8) 0.5550(8) 0.6373(6) 0.076(2) Uani 1 1 d . U . . . C24 C 0.1861(8) 0.5531(8) 0.6421(6) 0.0698(19) Uani 1 1 d . U . . . C25 C 0.2341(10) 0.4672(8) 0.6266(6) 0.079(2) Uani 1 1 d . U . . . C30 C 0.3882(9) 0.6296(9) 0.6601(7) 0.086(2) Uani 1 1 d D U . . . C6 C 0.4242(9) 0.8415(8) 0.8901(7) 0.078(2) Uani 1 1 d . U . . . Cl3 Cl 0.0305(17) 1.0361(11) 0.5826(14) 0.266(5) Uani 0.5 1 d . . P . . C12 C 0.2830(9) 0.7038(8) 0.9133(7) 0.077(2) Uani 1 1 d . U . . . C22 C -0.0547(9) 0.4638(10) 0.6117(7) 0.096(3) Uani 1 1 d . U . . . H22 H -0.048214 0.392349 0.596829 0.115 Uiso 1 1 calc R U . . . C5 C 0.4682(9) 0.9218(7) 0.8323(8) 0.080(2) Uani 1 1 d . U . . . C13 C 0.1681(12) 0.6103(10) 0.8986(9) 0.1126(6) Uani 1 1 d D U . . . C31 C 0.5200(15) 0.7049(16) 0.6940(13) 0.1103(10) Uani 0.687(8) 1 d D U P A 1 C7 C 0.4846(9) 0.8172(8) 0.9819(7) 0.084(2) Uani 1 1 d . U . . . C26 C 0.1974(11) 0.3490(8) 0.6054(6) 0.091(3) Uani 1 1 d . U . . . H26 H 0.113260 0.311088 0.598905 0.109 Uiso 1 1 calc R U . . . C4 C 0.5857(10) 0.9999(8) 0.8693(9) 0.099(3) Uani 1 1 d . U . . . H4 H 0.644414 1.005062 0.932722 0.119 Uiso 1 1 calc R U . . . C11 C 0.4129(12) 0.6812(10) 1.0765(7) 0.105(3) Uani 1 1 d . U . . . H11 H 0.350017 0.623261 1.082984 0.126 Uiso 1 1 calc R U . . . C19 C -0.0748(9) 0.6696(11) 0.6584(8) 0.102(3) Uani 1 1 d . U . . . H19 H -0.083194 0.739880 0.675293 0.122 Uiso 1 1 calc R U . . . C27 C 0.2804(12) 0.2911(10) 0.5945(8) 0.106(3) Uani 1 1 d . U . . . H27 H 0.254072 0.214187 0.580940 0.127 Uiso 1 1 calc R U . . . C1 C 0.4094(12) 0.9856(9) 0.6810(10) 0.105(3) Uani 1 1 d . U . . . H1 H 0.350496 0.981078 0.617823 0.126 Uiso 1 1 calc R U . . . C28 C 0.4141(13) 0.3503(10) 0.6041(9) 0.112(3) Uani 1 1 d . U . . . H28 H 0.471025 0.310668 0.594013 0.134 Uiso 1 1 calc R U . . . C8 C 0.6055(10) 0.8579(10) 1.0570(9) 0.105(3) Uani 1 1 d . U . . . H8 H 0.669228 0.915875 1.051565 0.126 Uiso 1 1 calc R U . . . C3 C 0.6111(13) 1.0728(10) 0.8031(12) 0.114(3) Uani 1 1 d . U . . . H3 H 0.690196 1.126451 0.823797 0.137 Uiso 1 1 calc R U . . . C32 C 0.5429(16) 0.7794(14) 0.6259(14) 0.1103(10) Uani 0.687(8) 1 d D U P A 1 H32 H 0.478464 0.774875 0.565073 0.132 Uiso 0.687(8) 1 calc R U P A 1 C21 C -0.1761(11) 0.4853(13) 0.6095(9) 0.117(4) Uani 1 1 d . U . . . H21 H -0.250513 0.426976 0.592928 0.140 Uiso 1 1 calc R U . . . C29 C 0.4535(11) 0.4599(10) 0.6271(8) 0.103(3) Uani 1 1 d . U . . . H29 H 0.538290 0.497034 0.634557 0.124 Uiso 1 1 calc R U . . . C20 C -0.1824(11) 0.5849(14) 0.6303(9) 0.115(4) Uani 1 1 d . U . . . H20 H -0.262323 0.598375 0.625820 0.138 Uiso 1 1 calc R U . . . C18 C 0.0444(16) 0.6482(14) 0.8990(13) 0.1126(6) Uani 0.761(2) 1 d D U P B 1 H18 H 0.045592 0.721949 0.913469 0.135 Uiso 0.761(2) 1 calc R U P B 1 C14 C 0.1593(17) 0.5059(14) 0.8876(14) 0.1126(6) Uani 0.761(2) 1 d D U P B 1 C2 C 0.5288(14) 1.0672(11) 0.7162(12) 0.121(4) Uani 1 1 d . U . . . H2 H 0.548431 1.117558 0.676260 0.145 Uiso 1 1 calc R U . . . C10 C 0.5329(13) 0.7219(12) 1.1501(9) 0.120(4) Uani 1 1 d . U . . . H10 H 0.551804 0.691197 1.207661 0.144 Uiso 1 1 calc R U . . . C9 C 0.6258(14) 0.8080(10) 1.1396(9) 0.122(4) Uani 1 1 d . U . . . H9 H 0.705826 0.833351 1.190921 0.146 Uiso 1 1 calc R U . . . C15 C 0.0380(18) 0.4177(15) 0.8720(13) 0.1126(6) Uani 0.761(2) 1 d D U P B 1 H15 H 0.034857 0.342726 0.865174 0.135 Uiso 0.761(2) 1 calc R U P B 1 C34 C 0.7532(16) 0.8529(15) 0.7483(14) 0.1103(10) Uani 0.687(8) 1 d D U P A 1 H34 H 0.834087 0.903902 0.767446 0.132 Uiso 0.687(8) 1 calc R U P A 1 C33 C 0.6622(17) 0.8570(15) 0.6531(13) 0.1103(10) Uani 0.687(8) 1 d D U P A 1 H33 H 0.681755 0.907539 0.613286 0.132 Uiso 0.687(8) 1 calc R U P A 1 C16 C -0.0609(16) 0.4537(13) 0.8688(14) 0.1126(6) Uani 0.761(2) 1 d D U P B 1 H16 H -0.136917 0.400216 0.860841 0.135 Uiso 0.761(2) 1 calc R U P B 1 C35 C 0.7383(15) 0.7888(15) 0.8104(15) 0.1103(10) Uani 0.687(8) 1 d D U P A 1 H35 H 0.802357 0.794425 0.871666 0.132 Uiso 0.687(8) 1 calc R U P A 1 C17 C -0.0692(17) 0.5610(13) 0.8755(13) 0.1126(6) Uani 0.761(2) 1 d D U P B 1 H17 H -0.149770 0.576421 0.864668 0.135 Uiso 0.761(2) 1 calc R U P B 1 Cl2 Cl 0.0044(17) 1.1293(11) 0.9135(14) 0.266(5) Uani 0.5 1 d . . P . . C36 C 0.6184(15) 0.7097(17) 0.7788(14) 0.1103(10) Uani 0.687(8) 1 d D U P A 1 Br4 Br 0.6171(7) 0.6463(7) 0.8369(6) 0.1103(10) Uani 0.313(8) 1 d D U P A 2 C2A C 0.609(2) 0.738(3) 0.743(2) 0.1103(10) Uani 0.313(8) 1 d D U P A 2 C37 C 0.728(3) 0.803(3) 0.751(3) 0.1103(10) Uani 0.313(8) 1 d D U P A 2 H37 H 0.805459 0.802235 0.799600 0.132 Uiso 0.313(8) 1 calc R U P A 2 C38 C 0.502(2) 0.713(3) 0.661(2) 0.1103(10) Uani 0.313(8) 1 d D U P A 2 C0 C 0.494(3) 0.786(3) 0.588(2) 0.1103(10) Uani 0.313(8) 1 d D U P A 2 H0 H 0.415397 0.781900 0.537401 0.132 Uiso 0.313(8) 1 calc R U P A 2 C39 C 0.609(3) 0.862(3) 0.595(3) 0.1103(10) Uani 0.313(8) 1 d D U P A 2 H39 H 0.615187 0.906427 0.548010 0.132 Uiso 0.313(8) 1 calc R U P A 2 C40 C 0.723(3) 0.866(3) 0.686(3) 0.1103(10) Uani 0.313(8) 1 d D U P A 2 H40 H 0.798681 0.920983 0.696473 0.132 Uiso 0.313(8) 1 calc R U P A 2 Cl Cl 0.1897(19) 0.8324(11) 0.3760(11) 0.141(7) Uani 0.345(17) 1 d . U P C 2 O3 O 0.1075(8) 0.9419(8) 0.9438(6) 0.141(4) Uani 1 1 d D . . . . H3A H 0.126(17) 0.916(12) 0.896(8) 0.211 Uiso 1 1 d D U . . . H3B H 0.084(19) 1.000(10) 0.924(12) 0.211 Uiso 1 1 d D U . . . C18A C 0.192(4) 0.492(3) 0.879(5) 0.1126(6) Uani 0.239(2) 1 d D U P B 2 H18A H 0.272459 0.482533 0.879570 0.135 Uiso 0.239(2) 1 calc R U P B 2 C14A C 0.052(3) 0.611(2) 0.888(4) 0.1126(6) Uani 0.239(2) 1 d D U P B 2 C15A C -0.058(4) 0.513(2) 0.876(4) 0.1126(6) Uani 0.239(2) 1 d D U P B 2 H15A H -0.138192 0.519399 0.878408 0.135 Uiso 0.239(2) 1 calc R U P B 2 C16A C -0.032(4) 0.421(3) 0.861(4) 0.1126(6) Uani 0.239(2) 1 d D U P B 2 H16A H -0.100355 0.358367 0.848780 0.135 Uiso 0.239(2) 1 calc R U P B 2 C17A C 0.084(4) 0.403(3) 0.862(4) 0.1126(6) Uani 0.239(2) 1 d D U P B 2 H17A H 0.090693 0.330838 0.851148 0.135 Uiso 0.239(2) 1 calc R U P B 2 Br2A Br 0.0525(5) 0.7522(4) 0.9427(4) 0.1126(6) Uani 0.239(2) 1 d D U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0637(7) 0.0816(8) 0.0729(8) 0.0079(6) 0.0253(5) 0.0190(6) Br1 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) Br2 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) Cl1 0.139(6) 0.173(6) 0.128(5) 0.038(4) 0.069(4) 0.028(5) N1 0.064(4) 0.104(5) 0.062(4) 0.021(4) 0.021(3) 0.019(4) N5 0.063(4) 0.078(4) 0.074(4) -0.002(3) 0.019(3) 0.023(3) N2 0.071(4) 0.072(4) 0.073(4) -0.008(3) 0.030(3) 0.006(3) O2 0.104(5) 0.116(5) 0.090(4) 0.024(4) 0.037(4) 0.054(4) O1 0.104(5) 0.133(6) 0.082(4) 0.035(4) 0.040(4) 0.028(4) N4 0.089(5) 0.073(5) 0.095(5) 0.008(4) 0.045(4) 0.027(4) N3 0.087(4) 0.088(4) 0.080(5) -0.010(4) 0.039(4) 0.021(3) N6 0.097(5) 0.081(5) 0.066(4) -0.002(3) 0.020(3) 0.039(4) C23 0.064(4) 0.100(5) 0.051(4) 0.005(4) 0.016(4) 0.006(4) C24 0.064(4) 0.080(5) 0.056(4) 0.002(4) 0.022(4) 0.000(3) C25 0.085(5) 0.085(5) 0.060(5) 0.001(4) 0.025(4) 0.014(4) C30 0.081(4) 0.092(5) 0.088(6) -0.015(5) 0.033(4) 0.030(4) C6 0.070(5) 0.070(5) 0.087(5) -0.008(4) 0.019(4) 0.021(4) Cl3 0.302(12) 0.181(8) 0.394(15) 0.116(9) 0.167(11) 0.130(8) C12 0.083(4) 0.081(5) 0.067(4) -0.002(4) 0.019(4) 0.037(4) C22 0.073(5) 0.117(7) 0.069(6) 0.004(5) 0.013(5) -0.012(5) C5 0.069(5) 0.062(5) 0.109(5) -0.004(4) 0.034(4) 0.021(4) C13 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) C31 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C7 0.073(5) 0.079(6) 0.089(5) -0.007(4) 0.010(4) 0.032(4) C26 0.100(6) 0.085(5) 0.062(5) 0.003(5) 0.005(5) 0.011(5) C4 0.073(5) 0.078(6) 0.140(8) -0.005(5) 0.033(5) 0.021(4) C11 0.135(8) 0.103(7) 0.064(5) 0.006(5) 0.008(5) 0.048(6) C19 0.062(5) 0.146(8) 0.094(7) 0.010(6) 0.025(5) 0.026(5) C27 0.123(7) 0.093(7) 0.087(7) -0.005(6) 0.029(6) 0.017(5) C1 0.113(7) 0.088(7) 0.145(8) 0.034(6) 0.073(6) 0.039(5) C28 0.129(7) 0.099(6) 0.110(8) -0.014(6) 0.052(7) 0.030(6) C8 0.079(5) 0.098(7) 0.113(7) -0.008(5) 0.003(5) 0.031(5) C3 0.094(7) 0.078(7) 0.175(10) 0.001(7) 0.065(6) 0.013(6) C32 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C21 0.072(6) 0.153(9) 0.101(8) 0.013(8) 0.025(6) -0.010(6) C29 0.103(7) 0.102(6) 0.113(8) -0.013(6) 0.050(6) 0.034(5) C20 0.074(6) 0.165(9) 0.094(7) 0.013(8) 0.026(5) 0.012(6) C18 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) C14 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) C2 0.124(9) 0.092(8) 0.162(10) 0.022(8) 0.074(7) 0.020(6) C10 0.136(8) 0.115(8) 0.093(7) 0.013(6) 0.002(6) 0.058(6) C9 0.124(8) 0.097(8) 0.103(7) -0.019(6) -0.011(6) 0.035(6) C15 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) C34 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C33 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C16 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) C35 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C17 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) Cl2 0.302(12) 0.181(8) 0.394(15) 0.116(9) 0.167(11) 0.130(8) C36 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) Br4 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C2A 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C37 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C38 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C0 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C39 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) C40 0.0913(11) 0.1304(19) 0.109(2) 0.0035(14) 0.0282(11) 0.0450(12) Cl 0.155(14) 0.136(9) 0.157(10) 0.039(7) 0.094(9) 0.022(8) O3 0.084(5) 0.183(9) 0.112(6) -0.085(6) 0.017(5) 0.009(5) C18A 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) C14A 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) C15A 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) C16A 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) C17A 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) Br2A 0.1180(11) 0.1074(11) 0.1147(11) -0.0028(8) 0.0337(9) 0.0518(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u -1 0 0 242.8 14.84 -1 0 0 280.46 14.88 -1 0 0 281.56 15.15 1 0 0 279.78 14.83 1 0 0 289.37 14.97 1 0 0 265.79 14.95 1 0 0 289.38 14.83 -2 0 0 28.09 2.43 -2 0 0 26.48 2.24 -2 0 0 29.65 2.4 -2 0 0 29.62 2.67 -2 0 0 26.91 2.13 2 0 0 29.13 2.62 2 0 0 30.35 2.51 2 0 0 28.46 2.49 2 0 0 25.27 2.09 2 0 0 29.03 2.28 2 0 0 28.27 2.18 -3 0 0 187.96 11.52 -3 0 0 191.69 11.71 -3 0 0 188.5 11.06 -3 0 0 207.16 11.33 -3 0 0 194.64 11.27 3 0 0 200.35 11.13 3 0 0 176.74 11.04 3 0 0 206.11 11.45 3 0 0 197.57 11.31 3 0 0 186.27 11.61 3 0 0 203.85 11.58 -4 0 0 85.65 5.97 -4 0 0 84.48 5.58 -4 0 0 83.77 6.37 -4 0 0 83.33 6.59 -4 0 0 75.72 5.77 4 0 0 85.57 5.64 4 0 0 73.96 5.78 4 0 0 77.71 6.31 4 0 0 88.57 5.77 4 0 0 90.94 6.29 4 0 0 80.39 6.21 -5 0 0 300.84 17.03 -5 0 0 278.28 16.58 -5 0 0 289.51 17.84 -5 0 0 294.04 17.55 -5 0 0 269.93 16.78 5 0 0 295.58 16.79 5 0 0 289.83 16.68 5 0 0 274.76 16.88 5 0 0 295.52 17.31 5 0 0 306.52 17.54 5 0 0 286.87 17.62 -6 0 0 123.55 8.78 -6 0 0 137.77 9.58 -6 0 0 130.38 10.57 -6 0 0 137.36 10.05 6 0 0 122.46 8.95 6 0 0 123.84 8.87 6 0 0 140.46 10.04 6 0 0 137.65 9.11 6 0 0 132.72 10.02 -7 0 0 31.46 3.77 -7 0 0 18.69 3.83 -7 0 0 29.41 4.8 -7 0 0 27.62 4.88 7 0 0 31.23 4.47 7 0 0 33.17 4.46 7 0 0 24.54 3.91 -8 0 0 16.52 3.68 -8 0 0 13.92 4.41 -8 0 0 27.91 5.67 8 0 0 10.86 4.17 8 0 0 19.81 4.32 -9 0 0 80.39 9.27 -9 0 0 53.3 7.55 -9 0 0 53.45 7.7 9 0 0 50.94 7.18 9 0 0 53.78 6.4 -10 0 0 19.74 6.99 -10 0 0 26.29 5.35 -10 0 0 22.17 6.51 10 0 0 22.42 5.83 10 0 0 18.17 6.02 -11 0 0 -0.54 6.11 -11 0 0 5.2 6.29 11 0 0 12.82 6.46 11 0 0 7.52 6.21 -12 0 0 5.33 6.77 12 0 0 11.82 6.86 12 -1 0 -1.95 5.94 12 -1 0 -7.54 6.28 -12 1 0 6.78 7.61 -12 1 0 1.7 6.8 11 -1 0 2.06 5.47 11 -1 0 -1.88 5.84 -11 1 0 0.29 6.46 -11 1 0 2.03 5.57 10 -1 0 7.59 4.33 10 -1 0 4.11 4.8 -10 1 0 9.57 6.44 -10 1 0 4.83 5.29 -10 1 0 3.73 4.23 9 -1 0 81.52 8.61 9 -1 0 39.94 6.56 -9 1 0 58.6 7.81 -9 1 0 57.21 7.36 -9 1 0 77.54 8.82 8 -1 0 84.61 9.69 8 -1 0 89.28 8.38 -8 1 0 84.88 10.05 -8 1 0 85.71 8.58 7 -1 0 48.88 5.8 7 -1 0 56.05 6.4 7 -1 0 56.32 5.68 -7 1 0 51.01 6.27 -7 1 0 61.97 6.61 -7 1 0 56.37 7.35 6 -1 0 28.95 3.52 6 -1 0 27.41 3.85 6 -1 0 26.02 3.83 6 -1 0 24.76 3.08 6 -1 0 19.03 2.73 -6 1 0 20.45 4.03 -6 1 0 26.46 4.13 -6 1 0 24.1 3.12 5 -1 0 124.66 9.26 5 -1 0 124.67 8.37 5 -1 0 135.3 8.56 5 -1 0 133.13 9.21 5 -1 0 131.94 8.4 5 -1 0 137.2 9.05 -5 1 0 124.52 8.3 -5 1 0 132.05 8.46 -5 1 0 122.02 9.22 -5 1 0 132.02 9.53 -5 1 0 116.35 8.38 4 -1 0 4.22 1.59 4 -1 0 3.84 1.26 4 -1 0 4.86 1.37 4 -1 0 4.51 1.42 4 -1 0 4.31 1.73 4 -1 0 7.05 1.83 -4 1 0 4.74 1.4 -4 1 0 6.46 1.5 -4 1 0 5.33 1.95 -4 1 0 7.21 1.45 -4 1 0 3.12 1.74 3 -1 0 24.34 2.46 3 -1 0 27.04 2.84 3 -1 0 20.72 2.28 3 -1 0 19.74 2.34 3 -1 0 17.35 2.36 3 -1 0 17.68 2.24 -3 1 0 17.23 2.34 -3 1 0 22.97 2.29 -3 1 0 25.98 2.57 -3 1 0 19.44 2.47 2 -1 0 298.08 16.1 2 -1 0 288.25 16.1 2 -1 0 298.7 16.4 2 -1 0 299.04 16.34 2 -1 0 283.82 15.94 2 -1 0 298.14 16.11 -2 1 0 290.48 16.07 -2 1 0 287.43 15.93 -2 1 0 291.35 16.08 -2 1 0 300.46 16.12 -2 1 0 289.17 16.39 -2 1 0 290.24 16.29 1 -1 0 554.46 29.48 1 -1 0 553.42 29.49 1 -1 0 533.23 29.64 1 -1 0 537.78 29.53 -1 1 0 595.42 29.41 -1 1 0 532.97 29.53 -1 1 0 548.59 29.65 -1 1 0 552.76 29.48 -1 1 0 549.89 29.44 -1 1 0 545.82 29.29 -1 1 0 552.74 29.49 -1 -1 0 523.8 27.81 -1 -1 0 514.78 27.74 -1 -1 0 520.12 27.54 -1 -1 0 515.62 27.62 -1 -1 0 500.66 27.52 1 1 0 525.03 27.74 1 1 0 519.46 27.64 1 1 0 498.77 27.51 1 1 0 493.35 27.73 1 1 0 522.35 27.56 1 1 0 518.61 27.39 -2 -1 0 2363.12 123.04 -2 -1 0 2312.69 122.73 -2 -1 0 2272.15 122.7 -2 -1 0 2359.41 122.46 -2 -1 0 2320.12 122.88 -2 -1 0 2291.77 122.48 2 1 0 2201.01 122.81 2 1 0 2338.92 122.48 2 1 0 2288.66 122.52 2 1 0 2354.69 122.78 2 1 0 2261.31 122.98 -3 -1 0 502.54 27.42 -3 -1 0 489.66 27.27 -3 -1 0 518.66 26.96 -3 -1 0 506.64 27.82 -3 -1 0 489.16 26.82 -3 -1 0 496.47 26.95 -3 -1 0 498.97 27.45 3 1 0 506.93 27.4 3 1 0 505.66 27.02 3 1 0 484.34 27.63 3 1 0 490.61 27.37 3 1 0 468.8 27.36 3 1 0 495.37 26.91 -4 -1 0 1.27 1.72 -4 -1 0 2.2 1.39 -4 -1 0 -0.32 1.17 -4 -1 0 -0.67 1.55 -4 -1 0 0.32 1.35 -4 -1 0 0.56 0.81 -4 -1 0 1.34 0.83 4 1 0 -1.13 1.12 4 1 0 2.1 1.31 4 1 0 -1.35 0.87 4 1 0 2.31 1.69 4 1 0 0.7 1.57 4 1 0 -0.02 1.53 4 1 0 0.27 1.15 -5 -1 0 9.14 2.15 -5 -1 0 12.19 1.5 -5 -1 0 11.75 3.02 -5 -1 0 12.79 2.79 -5 -1 0 8.96 2.27 -5 -1 0 9.99 1.97 -5 -1 0 12.46 1.74 5 1 0 12.85 2.21 5 1 0 10.25 2.2 5 1 0 11.77 2.53 5 1 0 16.02 2.96 5 1 0 8.68 2.14 5 1 0 12.42 2.58 5 1 0 13.3 1.7 -6 -1 0 0.77 1.31 -6 -1 0 -1.74 2.38 -6 -1 0 -0.3 2.49 -6 -1 0 2.76 2.08 -6 -1 0 0.92 1.26 -6 -1 0 1.62 1.9 6 1 0 0.33 1.39 6 1 0 -0.32 2.2 6 1 0 -1.52 1.5 6 1 0 0.41 1.85 6 1 0 4.32 2.84 6 1 0 -0.1 1.77 -7 -1 0 36.15 4.35 -7 -1 0 31.95 5.55 -7 -1 0 26.07 3.57 7 1 0 27.91 4.06 7 1 0 27.57 3.81 7 1 0 35.52 4.91 -8 -1 0 10.1 4.67 -8 -1 0 6.04 4.02 -8 -1 0 8.08 3.62 8 1 0 7.13 3.44 8 1 0 10.1 4.17 -9 -1 0 15.26 4.78 -9 -1 0 19.62 5.64 -9 -1 0 16.63 4.88 9 1 0 13.2 4.88 9 1 0 20.7 4.5 -10 -1 0 1.76 4.92 -10 -1 0 -0.97 5.24 -10 -1 0 6.61 4.95 10 1 0 1.49 4.77 10 1 0 8.69 5.89 -11 -1 0 12.59 6.33 -11 -1 0 6.36 7.27 11 1 0 -6.13 5.67 -12 -1 0 -0.67 7.24 12 1 0 -1.05 6.8 12 -2 0 24.8 7.3 12 -2 0 15.26 6.68 -12 2 0 11.52 8.15 -12 2 0 19.41 7.19 11 -2 0 12.83 5.88 11 -2 0 4.17 5.16 -11 2 0 14.89 6.59 -11 2 0 14.53 7.68 10 -2 0 7.44 4.33 10 -2 0 3.93 4.87 -10 2 0 9.36 5.77 -10 2 0 10.69 4.46 -10 2 0 15.94 6.21 9 -2 0 19.33 4.88 9 -2 0 13.03 4.16 -9 2 0 22.72 4.18 -9 2 0 12.45 5.17 -9 2 0 26.3 5.69 8 -2 0 1.14 2.99 8 -2 0 -3.93 3.25 -8 2 0 1.06 3.84 -8 2 0 3.98 2.84 -8 2 0 0.74 4.17 7 -2 0 128.63 10.45 7 -2 0 116.66 9.01 7 -2 0 130.45 9.65 -7 2 0 128.1 9.36 -7 2 0 133.99 10.85 -7 2 0 137.2 11.2 6 -2 0 49.14 5.31 6 -2 0 43.83 4.74 6 -2 0 53.52 6 6 -2 0 45.57 4.76 6 -2 0 35.49 4.91 -6 2 0 46.64 5.41 -6 2 0 48.12 4.63 -6 2 0 48.46 4.9 -6 2 0 63.06 6.63 5 -2 0 11.01 1.96 5 -2 0 15.66 2.43 5 -2 0 18.47 2.93 5 -2 0 15.87 2.92 5 -2 0 16.99 2.56 5 -2 0 15.4 2.86 -5 2 0 14.06 2.09 -5 2 0 12.53 2.88 -5 2 0 14.99 2.37 -5 2 0 14.4 2.36 -5 2 0 14.73 2.98 4 -2 0 8 1.98 4 -2 0 7.3 1.67 4 -2 0 8.4 1.4 4 -2 0 8.79 2.02 4 -2 0 7.17 1.68 4 -2 0 9.92 2.14 -4 2 0 8.2 1.43 -4 2 0 7.12 1.65 -4 2 0 7.12 2.11 -4 2 0 6.27 1.94 -4 2 0 8.33 1.52 3 -2 0 71.55 4.89 3 -2 0 79.36 5.27 3 -2 0 83.57 5.73 3 -2 0 78.59 5.31 3 -2 0 73.83 5.45 3 -2 0 78.9 5.15 -3 2 0 76.42 5.73 -3 2 0 75.39 5.17 -3 2 0 77.51 4.89 -3 2 0 79.52 5.26 -3 2 0 64.88 5.44 -3 2 0 81.41 5.17 2 -2 0 635.58 34.85 2 -2 0 635.96 34.29 2 -2 0 642.69 34.07 2 -2 0 641.24 34.64 2 -2 0 654.38 34.54 2 -2 0 656.9 34.44 2 -2 0 650.84 34.51 -2 2 0 626.49 34.4 -2 2 0 615.36 34.79 -2 2 0 644.13 34.51 -2 2 0 617.32 34.09 -2 2 0 663.08 34.33 -2 2 0 640.4 34.48 -2 2 0 620.33 34.58 1 -2 0 308.47 16.88 1 -2 0 300.24 16.81 1 -2 0 328.64 16.89 1 -2 0 315.16 16.94 1 -2 0 321.21 17.02 1 -2 0 307.11 16.9 1 -2 0 302.43 16.86 1 -2 0 320.6 17.17 -1 2 0 313.3 16.99 -1 2 0 299.38 17.1 -1 2 0 301.04 16.84 -1 2 0 307.02 16.91 -1 2 0 322.96 16.92 -1 2 0 304.45 16.86 0 -2 0 16.89 1.6 0 -2 0 15.02 1.53 0 -2 0 18.67 1.95 0 -2 0 16.55 1.29 0 -2 0 17.48 1.6 0 -2 0 16.08 1.72 0 -2 0 14.09 1.42 0 2 0 15 1.58 0 2 0 16.79 1.26 0 2 0 14.26 1.48 0 2 0 19.93 1.8 0 2 0 14.4 1.62 0 2 0 16.55 1.63 0 2 0 13.25 1.51 -1 -2 0 2465.93 131.74 -1 -2 0 2525.9 131.51 -1 -2 0 2403.49 131.48 -1 -2 0 2476.43 131.72 1 2 0 2491.46 131.53 1 2 0 2513.37 131.54 1 2 0 2418.03 131.69 1 2 0 2494.79 131.7 -2 -2 0 40.82 3.31 -2 -2 0 44.41 3.65 -2 -2 0 41.18 3.05 -2 -2 0 41.8 3.05 -2 -2 0 49.3 4.09 2 2 0 39.6 3.46 2 2 0 38.21 3.49 2 2 0 34.26 3.62 2 2 0 33.63 2.96 2 2 0 35.09 3.08 -3 -2 0 610.91 33.18 -3 -2 0 623.57 34.05 -3 -2 0 593.42 33.64 -3 -2 0 641.05 34.31 -3 -2 0 616.27 33.36 -3 -2 0 623.22 33.63 3 2 0 608.25 33.92 3 2 0 632.74 33.48 3 2 0 608.93 33.24 3 2 0 623.9 33.81 3 2 0 600.56 33.56 3 2 0 604.81 34.08 -4 -2 0 952.65 52.89 -4 -2 0 950 52.36 -4 -2 0 1022.71 52.63 -4 -2 0 998.46 53.67 -4 -2 0 992.95 53.34 -4 -2 0 1016.59 53.01 -4 -2 0 928.06 52.31 4 2 0 991.29 52.46 4 2 0 981.81 52.87 4 2 0 943.45 52.34 4 2 0 996.81 53.14 4 2 0 977.13 52.53 4 2 0 951.85 53.45 4 2 0 923.65 53.06 -5 -2 0 51.01 6.38 -5 -2 0 40.24 5.13 -5 -2 0 41.6 4.07 -5 -2 0 42.39 4.33 -5 -2 0 50.36 5.71 -5 -2 0 37.25 4.62 -5 -2 0 35.66 3.77 5 2 0 48.36 5.78 5 2 0 35.87 4.09 5 2 0 32.42 4.31 5 2 0 41.15 4.51 5 2 0 41.07 4.21 5 2 0 42.8 4.6 5 2 0 43.04 4.96 -6 -2 0 10.58 3.11 -6 -2 0 16.37 3.48 -6 -2 0 14.8 2.3 -6 -2 0 15.93 4.08 -6 -2 0 13.88 1.93 -6 -2 0 8.6 2.18 6 2 0 11.77 2.46 6 2 0 12.79 3.29 6 2 0 16.55 2.89 6 2 0 15.47 2.28 6 2 0 12.96 2.92 -7 -2 0 -0.14 2.81 -7 -2 0 0.98 3.36 -7 -2 0 -1.98 3.34 -7 -2 0 2.98 1.96 -7 -2 0 -6.45 1.94 7 2 0 0.62 2.7 7 2 0 -6.26 2.88 7 2 0 -1.6 3.16 7 2 0 -2.41 2.22 -8 -2 0 17.21 4.45 -8 -2 0 24.83 5.18 -8 -2 0 19.17 5.51 8 2 0 16.61 4.34 8 2 0 14.1 4.95 -9 -2 0 12.94 5.22 -9 -2 0 13.19 5.05 -9 -2 0 3.78 4.42 9 2 0 14.83 5.78 9 2 0 5.17 4.23 -10 -2 0 -0.83 5.65 -10 -2 0 13.81 5.75 10 2 0 -4.24 5.17 -11 -2 0 -4.83 5.08 -11 -2 0 5.32 5.91 11 2 0 9.21 6.2 12 -3 0 10.71 6.16 -12 3 0 6.74 8.85 -12 3 0 -3.49 5.86 11 -3 0 12.75 5.77 11 -3 0 -0.64 4.81 -11 3 0 17.78 6.36 -11 3 0 4.15 6.72 10 -3 0 15.87 4.73 10 -3 0 12.57 5.15 -10 3 0 8.83 4.01 -10 3 0 9.35 5.5 -10 3 0 21.79 6.72 9 -3 0 263.41 17.76 9 -3 0 264.29 18.34 -9 3 0 253.65 19.41 -9 3 0 281.83 19.32 -9 3 0 262.35 17.25 8 -3 0 47.17 5.99 8 -3 0 56.42 6.1 8 -3 0 65.93 7.31 -8 3 0 50.2 5.18 -8 3 0 72.57 9.13 7 -3 0 29.35 4.54 7 -3 0 18.5 3.67 7 -3 0 16.26 2.86 -7 3 0 27.74 4.5 -7 3 0 15.36 4.35 -7 3 0 23.14 3.17 6 -3 0 11.53 3.3 6 -3 0 8.42 5.15 6 -3 0 12.98 2.73 6 -3 0 12.48 2.99 6 -3 0 6.85 2.16 -6 3 0 8.83 1.92 -6 3 0 12.27 3.47 -6 3 0 9.96 3.2 5 -3 0 186.97 11.77 5 -3 0 194.4 12.06 5 -3 0 197.05 11.4 5 -3 0 191.74 11.84 5 -3 0 194.89 12.65 5 -3 0 185.71 12.27 -5 3 0 186.48 11.24 -5 3 0 180.25 11.61 -5 3 0 179.44 11.63 -5 3 0 197.61 12.82 -5 3 0 193.54 12.4 4 -3 0 134.2 8.28 4 -3 0 116.79 7.79 4 -3 0 125.26 8.78 4 -3 0 126.35 8.54 4 -3 0 123.91 8.15 4 -3 0 130.3 8.3 -4 3 0 128.37 8.62 -4 3 0 118.69 7.81 -4 3 0 134.33 9.02 -4 3 0 122.89 8.02 -4 3 0 134.83 8.34 3 -3 0 49.88 3.81 3 -3 0 57.16 4.29 3 -3 0 56.96 4.19 3 -3 0 58.63 4.3 3 -3 0 46.68 4.54 3 -3 0 53.1 3.3 3 -3 0 44.71 4.06 3 -3 0 55.59 4.46 -3 3 0 53.39 3.96 -3 3 0 54.38 4.42 -3 3 0 46.63 4.58 -3 3 0 52.69 4.04 -3 3 0 50.38 4.24 2 -3 0 401.15 21.72 2 -3 0 409.54 22.18 2 -3 0 407.25 21.76 2 -3 0 402.25 21.56 2 -3 0 391.57 21.36 2 -3 0 393.4 21.55 2 -3 0 367.52 21.77 2 -3 0 396.09 21.62 -2 3 0 389.09 22.05 -2 3 0 367.62 21.54 -2 3 0 398.85 21.79 -2 3 0 400.26 21.57 -2 3 0 384.21 21.41 -2 3 0 394.95 21.7 -2 3 0 411.56 21.62 1 -3 0 102.67 6.15 1 -3 0 108.79 6.53 1 -3 0 107.54 6.31 1 -3 0 98.56 6.35 1 -3 0 99.7 6.39 1 -3 0 96.55 6.1 1 -3 0 104.54 6.11 1 -3 0 93.08 6.01 -1 3 0 103.47 6.12 -1 3 0 95.83 6.05 -1 3 0 107.6 6.28 -1 3 0 108.49 6.44 -1 3 0 102.3 6.15 0 -3 0 365.74 20.76 0 -3 0 380.08 20.72 0 -3 0 376.8 20.72 0 -3 0 394.03 21.06 0 -3 0 374.54 20.84 0 -3 0 372.6 20.46 0 -3 0 415.3 21.04 0 3 0 375.31 20.74 0 3 0 387.96 21.03 0 3 0 372.56 20.88 0 3 0 364.68 20.44 0 3 0 370.15 20.82 0 3 0 381.97 20.89 0 3 0 378.03 20.71 -1 -3 0 1200.31 63.07 -1 -3 0 1189.47 62.73 -1 -3 0 1111.14 62.65 -1 -3 0 1215.56 63.05 -1 -3 0 1195.6 62.91 1 3 0 1159.01 62.91 1 3 0 1203.06 62.96 1 3 0 1078.1 62.67 1 3 0 1178.45 62.78 -2 -3 0 1428.35 74.95 -2 -3 0 1341.54 74.41 -2 -3 0 1423.79 74.92 -2 -3 0 1424.61 74.39 2 3 0 1431.17 74.6 2 3 0 1402.58 74.48 2 3 0 1325.32 74.7 2 3 0 1328.79 74.73 -3 -3 0 617.36 32.66 -3 -3 0 574.58 32.01 -3 -3 0 593.96 32.77 -3 -3 0 594.23 31.8 3 3 0 548.02 32.25 3 3 0 580.59 31.92 3 3 0 593.3 32.2 3 3 0 547.92 32.34 -4 -3 0 96.83 6.63 -4 -3 0 120.42 7.53 -4 -3 0 109.36 7.51 -4 -3 0 106.56 7.51 -4 -3 0 102.8 8.59 -4 -3 0 101.2 6.96 -4 -3 0 108.71 8.32 4 3 0 94.38 7.6 4 3 0 116.03 8.31 4 3 0 108.48 6.82 4 3 0 105.18 7.4 4 3 0 106.68 8.32 4 3 0 98.12 7.25 -5 -3 0 0.7 1.61 -5 -3 0 -0.92 1.29 -5 -3 0 1.7 2.12 -5 -3 0 -1.56 1.4 -5 -3 0 3.69 2.94 -5 -3 0 -0.12 2.23 5 3 0 0.89 1.71 5 3 0 2.11 2.13 5 3 0 3.64 1.81 5 3 0 1.6 1.68 5 3 0 2.13 1.78 5 3 0 -1.27 2.49 -6 -3 0 171.36 10.67 -6 -3 0 159.43 11.18 -6 -3 0 153.78 11.91 -6 -3 0 137.85 9.94 -6 -3 0 165.53 12.99 6 3 0 156.9 10.9 6 3 0 153.97 10.29 6 3 0 169.14 12.13 6 3 0 153.56 10.17 6 3 0 143.22 9.99 -7 -3 0 1.26 3.33 -7 -3 0 0.95 3.78 -7 -3 0 6.79 3.37 -7 -3 0 1.28 2.2 7 3 0 5.03 2.24 7 3 0 4.99 4.02 7 3 0 4.74 2.96 -8 -3 0 8.25 4.27 -8 -3 0 8.2 4.17 -8 -3 0 12.65 5.73 8 3 0 12.5 4.87 8 3 0 0.68 3.31 -9 -3 0 1.62 5.58 -9 -3 0 4.44 4.64 9 3 0 -0.96 5.14 -10 -3 0 5.01 5.96 -10 -3 0 2.55 6.18 10 3 0 4.24 6.3 -11 -3 0 4.41 7.24 -11 -3 0 -6.99 6.62 11 3 0 0.08 7.23 12 -4 0 7.46 5.56 12 -4 0 5.05 5.85 -12 4 0 -1.71 6.51 -12 4 0 10.92 8.06 11 -4 0 -2.3 4.47 11 -4 0 2.26 5 -11 4 0 -2.59 6.75 -11 4 0 2.39 5.42 10 -4 0 -2.2 3.98 10 -4 0 -4.17 4.22 -10 4 0 1 5.88 -10 4 0 0.2 4.74 9 -4 0 19.12 4.91 9 -4 0 13.64 4.38 -9 4 0 7.91 3.67 -9 4 0 20.44 5.16 -9 4 0 12 5.46 8 -4 0 147.71 11.21 8 -4 0 114 11.3 8 -4 0 147.06 11.76 -8 4 0 152.3 12.66 -8 4 0 155.83 12.83 -8 4 0 149.79 10.44 7 -4 0 3.48 2.73 7 -4 0 7.63 2.98 7 -4 0 1.02 1.88 -7 4 0 3.62 1.95 -7 4 0 5.32 3.7 -7 4 0 3.1 3.27 6 -4 0 400.85 23.37 6 -4 0 387.01 22.71 6 -4 0 388.95 23.25 -6 4 0 398.06 22.57 -6 4 0 413.65 24.38 -6 4 0 410.22 23.83 5 -4 0 69.53 5.91 5 -4 0 66.51 6.39 5 -4 0 69.99 6.7 5 -4 0 64.65 5.42 5 -4 0 68.37 6.38 5 -4 0 73.79 6.11 -5 4 0 70.27 5.77 -5 4 0 73.52 6.22 -5 4 0 77.63 5.8 -5 4 0 80.29 6.93 -5 4 0 72.6 7.17 4 -4 0 34.15 2.42 4 -4 0 36.76 4 4 -4 0 35.82 4.3 4 -4 0 27.05 3.23 4 -4 0 29.12 3.59 4 -4 0 33.61 4.15 4 -4 0 32.48 3.75 4 -4 0 33.98 4.2 -4 4 0 34.89 3.93 -4 4 0 26.88 3.25 -4 4 0 38.34 4.69 -4 4 0 26.66 3.45 -4 4 0 22.81 2.83 3 -4 0 64.38 4.23 3 -4 0 61.48 5.38 3 -4 0 61.52 4.8 3 -4 0 61.26 5.27 3 -4 0 73.33 5.11 3 -4 0 69.78 4.99 3 -4 0 67.42 4.91 3 -4 0 60.29 4.66 -3 4 0 61.52 5.6 -3 4 0 58.58 4.73 -3 4 0 66.23 4.43 -3 4 0 63.55 4.92 -3 4 0 67.39 5.04 -3 4 0 66.3 5.32 2 -4 0 129.9 7.65 2 -4 0 125.06 7.94 2 -4 0 135.43 7.97 2 -4 0 122.97 8.34 2 -4 0 128.85 7.99 2 -4 0 135.75 7.93 2 -4 0 130.14 8.15 2 -4 0 124.65 7.84 -2 4 0 132.85 7.99 -2 4 0 125.74 7.9 -2 4 0 134.62 8.24 -2 4 0 130.53 7.87 -2 4 0 118.82 7.71 1 -4 0 4.21 1.28 1 -4 0 5.51 1.25 1 -4 0 6.67 1.67 1 -4 0 5.84 1.29 1 -4 0 4.53 1.16 1 -4 0 2.42 0.89 1 -4 0 5.02 1.41 1 -4 0 2.02 1.51 1 -4 0 6.47 1.52 -1 4 0 6.29 1.42 -1 4 0 4.86 1.26 -1 4 0 3.8 1.07 -1 4 0 2.48 1.21 -1 4 0 4.76 1.58 0 -4 0 4.98 1.63 0 -4 0 6.88 1.45 0 -4 0 3.59 1.48 0 -4 0 4.74 1.21 0 -4 0 4.28 0.95 0 -4 0 3.07 1.11 0 -4 0 3.33 1.03 0 -4 0 2.53 1.42 0 4 0 2.96 1.65 0 4 0 2.86 1.26 0 4 0 5.6 1.35 0 4 0 4.99 1.09 0 4 0 6.98 1.14 0 4 0 5.77 1.43 0 4 0 2.69 1.33 -1 -4 0 1.29 1.15 -1 -4 0 3.86 1.97 -1 -4 0 1.52 1.53 -1 -4 0 2.19 1 -1 -4 0 2.07 1.32 1 4 0 2.14 1.26 1 4 0 3.22 1.16 1 4 0 1.88 1.52 1 4 0 3.11 1.46 -2 -4 0 1008.25 56.42 -2 -4 0 1037.39 56.41 -2 -4 0 1101.21 57.13 -2 -4 0 1080.37 57.09 2 4 0 989.47 56.7 2 4 0 1040.69 56.56 2 4 0 993.46 56.76 2 4 0 1107.12 56.64 -3 -4 0 3.04 1.85 -3 -4 0 7.82 2.54 -3 -4 0 1.38 2.08 -3 -4 0 6.07 1.83 -3 -4 0 5.5 1.61 3 4 0 4.59 1.62 3 4 0 7.75 2.37 3 4 0 0.61 2.43 3 4 0 3.2 1.82 -4 -4 0 425.36 24.78 -4 -4 0 469.69 25.86 -4 -4 0 395.72 24.38 -4 -4 0 443.56 26 -4 -4 0 457.93 24.98 4 4 0 401.48 25.1 4 4 0 404.2 25.21 4 4 0 484.49 25.48 4 4 0 450.77 24.78 -5 -4 0 30.01 3.6 -5 -4 0 41.06 4.95 -5 -4 0 21.05 2.9 -5 -4 0 42.47 5.38 -5 -4 0 31.75 4.73 -5 -4 0 27.75 2.96 5 4 0 24.64 3.45 5 4 0 37.01 4.52 5 4 0 29.36 3.39 -6 -4 0 15.29 3.53 -6 -4 0 19 4.33 -6 -4 0 12.93 2.81 -6 -4 0 8.77 3.92 6 4 0 9.81 2.81 6 4 0 27.01 4.61 6 4 0 13.39 2.92 -7 -4 0 19.13 3.51 -7 -4 0 19.78 4.74 -7 -4 0 38.21 6.47 -7 -4 0 22.54 4.46 7 4 0 25.55 5.78 7 4 0 25.32 4.99 7 4 0 20.68 3.27 -8 -4 0 2.13 4.6 -8 -4 0 4.04 4.87 -8 -4 0 -0.5 3.05 8 4 0 6.79 5.11 -9 -4 0 16.52 6.44 -9 -4 0 13.3 5.8 9 4 0 5.82 5.73 -10 -4 0 0.57 6.5 -10 -4 0 10.86 6.86 10 4 0 -2.17 6.62 -11 -4 0 -2.62 7.56 -11 -4 0 -4.02 6.78 11 4 0 4.99 8.05 12 -5 0 3.82 6.12 12 -5 0 -2.03 5.5 -12 5 0 9.66 7.89 -12 5 0 -1.69 5.85 11 -5 0 20.34 6.1 11 -5 0 18.41 5.9 -11 5 0 19.68 7.43 -11 5 0 19.58 6.81 10 -5 0 28.78 5.67 10 -5 0 43.35 6.53 -10 5 0 27.31 6.08 -10 5 0 32.17 7.28 9 -5 0 -1 3.68 9 -5 0 1.33 4.33 -9 5 0 -1.09 3.18 -9 5 0 3.54 4.31 -9 5 0 3.54 5.06 8 -5 0 7.4 3.53 8 -5 0 7.53 3.65 -8 5 0 1.59 2.82 -8 5 0 9.03 4.31 -8 5 0 7.74 4.87 7 -5 0 61.82 7.1 7 -5 0 62.02 7.44 -7 5 0 54.46 7.11 -7 5 0 68.17 6.61 -7 5 0 70.7 8.6 6 -5 0 433.04 24.23 6 -5 0 404.38 23.59 6 -5 0 409.9 24.17 -6 5 0 422.92 25.31 -6 5 0 398.63 23.55 -6 5 0 422.17 24.72 5 -5 0 445.53 23.48 5 -5 0 413.42 23.55 5 -5 0 398.09 23.26 5 -5 0 393.82 23.76 5 -5 0 419.48 23.54 5 -5 0 388.19 24.34 5 -5 0 382.67 22.88 -5 5 0 410.9 23.06 -5 5 0 424.61 24.51 -5 5 0 425.44 23.86 -5 5 0 364.8 23.07 -5 5 0 426.42 23.61 4 -5 0 298.47 18.25 4 -5 0 283.65 16.97 4 -5 0 292.17 16.53 4 -5 0 315.24 16.86 4 -5 0 281.97 17.75 4 -5 0 293.66 17.26 4 -5 0 323.6 17.61 4 -5 0 318.42 17.41 4 -5 0 288.31 17.49 -4 5 0 298.47 17.22 -4 5 0 309.58 17.79 -4 5 0 308.28 17.53 -4 5 0 274.24 17.11 -4 5 0 292.92 18.16 -4 5 0 298.73 16.75 3 -5 0 345.75 18.83 3 -5 0 325.81 19.28 3 -5 0 334.65 19.08 3 -5 0 339.72 19.12 3 -5 0 318.45 19.88 3 -5 0 326.56 19.2 3 -5 0 344.37 19.64 3 -5 0 353.03 19.38 -3 5 0 331.51 19.01 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7.96 -2 -5 0 91.31 7.21 -2 -5 0 98.4 6.81 -2 -5 0 85.52 6.72 2 5 0 94.07 6.94 2 5 0 92.24 7.19 2 5 0 93.2 7.42 2 5 0 100.17 7.53 -3 -5 0 0.79 1.93 -3 -5 0 -0.11 2.41 -3 -5 0 3.15 2.74 -3 -5 0 -0.23 1.58 -3 -5 0 0.23 1.55 3 5 0 -1.03 2.5 3 5 0 0.1 2.37 3 5 0 3.22 1.85 3 5 0 -0.99 1.99 -4 -5 0 4.56 2.16 -4 -5 0 9.95 2.61 -4 -5 0 11.91 3.5 -4 -5 0 14.63 3.48 4 5 0 11.35 2.54 4 5 0 11.88 3.45 -5 -5 0 79.8 9.52 -5 -5 0 79.67 8.93 -5 -5 0 66.48 7.21 5 5 0 92.02 9.07 5 5 0 77.7 7.42 -6 -5 0 18.42 3.44 -6 -5 0 24.53 4.91 -6 -5 0 22.34 5.25 6 5 0 26.31 3.94 6 5 0 16.57 4.89 -7 -5 0 25.65 5.67 -7 -5 0 17.96 6.05 -7 -5 0 8.28 3.25 7 5 0 13.01 5.53 7 5 0 12.05 3.28 -8 -5 0 12.88 6.33 -8 -5 0 4.5 3.53 -8 -5 0 10.34 5.14 8 5 0 9.29 5.5 -9 -5 0 0.92 6.31 -9 -5 0 1.61 5.78 9 5 0 -5.24 5.27 -10 -5 0 7.11 7.89 -10 -5 0 -6.76 6.55 10 5 0 -4.83 6.51 12 -6 0 8.7 6.49 12 -6 0 12.55 6.5 -12 6 0 7.15 7.95 -12 6 0 -1.45 6.92 11 -6 0 -0.2 5.23 11 -6 0 -0.59 4.99 -11 6 0 -1.33 6.21 -11 6 0 5.35 6.21 10 -6 0 16.72 5.42 10 -6 0 12.85 4.67 -10 6 0 11.99 6.33 -10 6 0 10.05 6.39 9 -6 0 2.51 3.86 9 -6 0 6.86 3.99 -9 6 0 4.02 5 -9 6 0 4.12 3.5 -9 6 0 -2.27 5.1 8 -6 0 86.05 8.91 8 -6 0 91.26 9.69 -8 6 0 82.53 8.58 -8 6 0 96.52 11.03 -8 6 0 102.16 11.62 7 -6 0 66.65 8.31 7 -6 0 70.42 8.05 -7 6 0 68.85 7.46 -7 6 0 89.82 10.03 -7 6 0 80.17 9.18 6 -6 0 38.19 4.6 6 -6 0 41.01 4.9 6 -6 0 29.65 3.61 -6 6 0 47.97 5.65 -6 6 0 39.56 5.88 5 -6 0 1.98 1.46 5 -6 0 -3.52 1.8 5 -6 0 -1.5 1.65 5 -6 0 1.55 2.39 5 -6 0 4.09 2.39 5 -6 0 -2.33 1.98 5 -6 0 0.96 1.01 -5 6 0 2.68 2.96 -5 6 0 0.44 1.87 -5 6 0 2.9 2.15 -5 6 0 5.21 3.12 -5 6 0 3.23 1.55 -5 6 0 4.07 2.24 4 -6 0 19.99 2.44 4 -6 0 22.56 3.02 4 -6 0 18.22 2.84 4 -6 0 15.06 3.1 4 -6 0 26.75 3.46 4 -6 0 21.78 2.91 4 -6 0 22.75 3.56 4 -6 0 14.62 2.46 4 -6 0 17.77 2.05 -4 6 0 28.59 3.25 -4 6 0 22.15 2.52 -4 6 0 23.36 3.47 -4 6 0 24.59 3.37 3 -6 0 606.46 33.99 3 -6 0 655.09 34.46 3 -6 0 613.31 35.16 3 -6 0 649.72 35.25 3 -6 0 623.01 34.46 3 -6 0 580.48 34.57 3 -6 0 592.15 34.17 3 -6 0 568.9 34.21 3 -6 0 662.39 34.28 -3 6 0 652.96 34.8 -3 6 0 607.39 34.34 -3 6 0 628.95 34.26 -3 6 0 632.6 34.45 -3 6 0 634.48 34.25 2 -6 0 5.35 1.94 2 -6 0 1.7 1.71 2 -6 0 2.32 1.31 2 -6 0 3.86 2.04 2 -6 0 3.67 1.56 2 -6 0 3.82 2.15 2 -6 0 4.18 1.98 2 -6 0 4.86 1.66 2 -6 0 3.62 1.91 2 -6 0 3.77 2.4 -2 6 0 4.96 1.84 -2 6 0 2.84 1.96 -2 6 0 5.35 1.71 -2 6 0 2.48 1.7 -2 6 0 2.34 2.5 1 -6 0 462.79 26.08 1 -6 0 465.4 26.2 1 -6 0 441.44 25.85 1 -6 0 488.65 26.51 1 -6 0 445.92 25.78 1 -6 0 518.86 26.82 1 -6 0 458.03 26.11 1 -6 0 460.37 25.66 1 -6 0 436.05 25.97 -1 6 0 497.9 25.9 -1 6 0 465.74 25.6 -1 6 0 449.8 26.21 -1 6 0 449.27 26.09 0 -6 0 28.27 3.83 0 -6 0 34.82 4.25 0 -6 0 26.99 3.13 0 -6 0 23.13 2.86 0 -6 0 21.72 3.56 0 -6 0 29.23 3 0 -6 0 21.45 3.05 0 6 0 30.65 3.16 0 6 0 28.36 3.25 0 6 0 22.63 3.36 0 6 0 23.15 2.91 -1 -6 0 182.04 12.03 -1 -6 0 175.08 11.73 -1 -6 0 161.87 10.58 -1 -6 0 170.2 10.68 -1 -6 0 163.29 10.92 1 6 0 159.36 10.95 1 6 0 179.43 11.14 1 6 0 171.91 11.11 1 6 0 166.37 11.34 -2 -6 0 1.66 2.05 -2 -6 0 3.13 2.82 -2 -6 0 -2.93 1.6 -2 -6 0 -1.33 2.12 2 6 0 1.48 2.18 2 6 0 1.97 1.73 2 6 0 4.4 2.51 -3 -6 0 128.1 9.64 -3 -6 0 105.16 8.67 -3 -6 0 141.2 11.09 -3 -6 0 134.57 10.66 3 6 0 141.14 10.3 3 6 0 118.58 9.05 -4 -6 0 -0.07 2.23 -4 -6 0 -0.86 4.05 -4 -6 0 0.37 3.4 4 6 0 1.62 3.03 4 6 0 -2.78 1.98 -5 -6 0 17.79 5.06 -5 -6 0 17 3.85 -5 -6 0 8.54 2.84 5 6 0 14.77 3.16 5 6 0 25.45 4.76 -6 -6 0 7.52 5.22 -6 -6 0 -0.09 3.04 -6 -6 0 2.67 4.33 6 6 0 5.32 2.96 6 6 0 1.59 4.32 -7 -6 0 7.14 5.95 -7 -6 0 4.96 5.04 -7 -6 0 1.76 3.19 7 6 0 10.28 5.72 7 6 0 10.06 3.72 -8 -6 0 11.88 5.97 -8 -6 0 2.69 4.12 -8 -6 0 12.9 7.66 8 6 0 5.56 6.12 8 6 0 1.57 3.84 -9 -6 0 2.74 7.16 -9 -6 0 7 5.95 9 6 0 1.09 6.88 -10 -6 0 -1.49 7.31 -10 -6 0 6.71 8.6 10 6 0 8.73 7.88 12 -7 0 -3.08 6.17 12 -7 0 4.95 5.83 -12 7 0 7.35 7.48 11 -7 0 -3.22 5.08 11 -7 0 -6.35 5.27 -11 7 0 5.45 6.43 -11 7 0 3.77 6.23 10 -7 0 -3.26 5.11 10 -7 0 -2.71 4.2 -10 7 0 3.11 5.66 -10 7 0 -0.04 5.83 9 -7 0 0.18 3.87 9 -7 0 -2.82 3.65 -9 7 0 -1.2 4.8 -9 7 0 -0.57 4.76 8 -7 0 18.7 4.7 8 -7 0 20.1 4.78 -8 7 0 24.49 4.05 -8 7 0 15.94 5.18 -8 7 0 13.86 5.39 7 -7 0 155.48 11.58 7 -7 0 159.57 11.6 -7 7 0 137.44 12.25 -7 7 0 128.66 10.77 -7 7 0 146.02 13.12 6 -7 0 6.65 2.88 6 -7 0 5.93 1.38 6 -7 0 10.75 3.41 6 -7 0 5.86 1.84 -6 7 0 6.03 3.69 -6 7 0 8.44 4.18 -6 7 0 7.15 2.03 -6 7 0 11.22 3.09 5 -7 0 84.65 6.33 5 -7 0 100.68 8.14 5 -7 0 93.37 8.1 5 -7 0 109.59 7.12 -5 7 0 101.51 7.4 -5 7 0 97.25 8.06 -5 7 0 88.13 8.16 -5 7 0 90.33 9 4 -7 0 207.53 14.53 4 -7 0 208.57 12.76 4 -7 0 187.54 13.13 4 -7 0 212.07 13.4 4 -7 0 235.47 13.43 4 -7 0 206.88 14.95 4 -7 0 212.34 13.56 4 -7 0 195.56 13.69 4 -7 0 240.19 13.96 -4 7 0 213.13 13.66 -4 7 0 221.56 13.75 -4 7 0 242.87 14.43 -4 7 0 225.26 13.38 3 -7 0 1.9 1.59 3 -7 0 0.02 2.01 3 -7 0 -2.17 1.64 3 -7 0 -1.67 1.97 3 -7 0 2.6 1.99 3 -7 0 -2.42 1.51 3 -7 0 2.3 2.99 3 -7 0 0.13 2.01 3 -7 0 -2.03 1.85 3 -7 0 3.08 2.94 -3 7 0 1.33 2.34 -3 7 0 8.07 2.3 -3 7 0 2.04 2.86 -3 7 0 0.57 2.13 -3 7 0 -1.57 1.57 2 -7 0 58.52 5.32 2 -7 0 50.67 5.45 2 -7 0 62.38 6.94 2 -7 0 71.52 6.66 2 -7 0 67.9 6.5 2 -7 0 57.52 5.19 2 -7 0 64.13 5.39 2 -7 0 46.68 5.17 2 -7 0 59.54 5.14 2 -7 0 53.66 5.7 -2 7 0 61.99 5.79 -2 7 0 59.89 6.15 -2 7 0 64.24 6.79 -2 7 0 55.25 5.29 -2 7 0 61.14 6.14 1 -7 0 35.05 4.48 1 -7 0 23.85 3.04 1 -7 0 30.22 3.7 1 -7 0 26.9 3.76 1 -7 0 34.74 3.99 1 -7 0 35.96 4.34 1 -7 0 24.59 3.01 1 -7 0 23.96 3.31 1 -7 0 24.18 2.84 -1 7 0 34.17 3.75 -1 7 0 32.21 3.9 -1 7 0 31.47 3.78 -1 7 0 21.8 3.13 0 -7 0 218.47 13.35 0 -7 0 211.64 13.84 0 -7 0 250.12 15.24 0 -7 0 228.33 14.36 0 -7 0 235.17 15.19 0 -7 0 230.84 14.18 0 7 0 227.66 14.65 0 7 0 238.81 13.36 0 7 0 259.73 14.53 0 7 0 219.28 14.42 -1 -7 0 3.3 2.42 -1 -7 0 0.97 1.79 -1 -7 0 -0.43 3.39 -1 -7 0 2.9 2.23 1 7 0 0.9 2.18 1 7 0 2.15 2.68 1 7 0 2.95 2.14 -2 -7 0 65.39 7.18 -2 -7 0 49.17 6.32 -2 -7 0 55.71 5.86 -2 -7 0 65.94 7.84 2 7 0 76.7 7.32 2 7 0 72.41 6.9 -3 -7 0 70.57 9.33 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3.38 1 -8 0 10.98 2.83 1 -8 0 9.21 2.77 1 -8 0 10.62 3.71 1 -8 0 8.06 2.41 1 -8 0 9.34 2.62 -1 8 0 6.93 2.62 -1 8 0 12.42 2.4 -1 8 0 12.53 3 0 -8 0 2.43 2.08 0 -8 0 15.04 3.82 0 -8 0 10.51 2.9 0 -8 0 11.33 3.85 0 -8 0 6.79 2.81 0 -8 0 5.25 2.06 0 -8 0 6.3 2.21 0 -8 0 12.72 2.28 0 8 0 7.97 2.67 0 8 0 10.51 3.59 -1 -8 0 70.27 8.03 -1 -8 0 48.23 5.78 -1 -8 0 71.41 7.62 -1 -8 0 42.29 6.47 1 8 0 71.5 7.76 1 8 0 62.3 6.79 -2 -8 0 8.48 3.17 -2 -8 0 -1.54 4.26 -2 -8 0 6.4 4.02 2 8 0 3.65 3.54 2 8 0 7.18 2.76 -3 -8 0 13.39 4.73 -3 -8 0 5.92 5.15 -3 -8 0 10.97 3.67 3 8 0 11.1 3.25 3 8 0 10.42 4.2 -4 -8 0 2.61 4.14 -4 -8 0 4.73 3.39 -4 -8 0 4.56 5.58 4 8 0 10.47 4.65 4 8 0 1.25 2.88 -5 -8 0 5.47 3.67 -5 -8 0 -0.06 5.03 -5 -8 0 -2.12 5.52 5 8 0 3.86 4.48 5 8 0 -0.17 3.2 -6 -8 0 16.36 7.2 -6 -8 0 18 6.23 -6 -8 0 14.23 4.35 6 8 0 12.17 4.24 6 8 0 18.84 6.19 -7 -8 0 7.44 7.54 -7 -8 0 -0.8 5.48 -7 -8 0 0.4 4.27 7 8 0 -11.21 5.96 7 8 0 -4.26 3.76 -8 -8 0 1.82 8.4 -8 -8 0 1.33 6.27 -8 -8 0 -5.63 4.9 8 8 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16 10.49 8.65 -8 -1 16 -5.35 6.33 7 1 -16 -2.93 4.42 -7 -1 16 3.62 6.94 -7 -1 16 3.4 8.79 6 1 -16 -5.61 3.69 -6 -1 16 1.3 6.84 -6 -1 16 -5.66 6.43 5 1 -16 -0.58 3.53 -5 -1 16 0.14 5.78 -5 -1 16 3.06 6.25 4 1 -16 4.33 3.73 -4 -1 16 7.26 6.6 -4 -1 16 8.41 6.31 3 1 -16 1.08 5.12 3 1 -16 3.66 4.18 -3 -1 16 0.84 6.7 -3 -1 16 -5.14 5.82 2 1 -16 8.46 5.86 2 1 -16 3.39 4.29 -2 -1 16 8.02 6.33 -2 -1 16 6.35 7.28 1 1 -16 -3.15 5.09 1 1 -16 6.25 4.71 -1 -1 16 -3.34 6.46 -1 -1 16 1.38 7.09 0 1 -16 -9.23 4.47 0 1 -16 -5.21 5.23 0 -1 16 2.67 6.25 -1 1 -16 -4.77 5.03 -1 1 -16 -2.24 5.63 1 -1 16 -0.44 6.87 9 0 -16 1.74 5.02 -9 0 16 0.41 9.11 -9 0 16 -4.94 6.5 8 0 -16 -6.81 4.64 -8 0 16 -6.71 8.64 -8 0 16 6.47 6.97 7 0 -16 -2.42 4.03 -7 0 16 5.02 9.02 -7 0 16 -0.4 6.09 6 0 -16 6.35 4.25 -6 0 16 4.23 6.57 -6 0 16 6.59 6.28 5 0 -16 5.65 4.1 -5 0 16 -9.28 6.3 -5 0 16 1.22 6.21 4 0 -16 10.82 4.59 -4 0 16 2.65 6.81 -4 0 16 9.68 5.97 3 0 -16 -1.15 3.46 -3 0 16 -2.53 6.11 -3 0 16 4.95 6.48 2 0 -16 -1.68 4.8 2 0 -16 -2.47 3.87 -2 0 16 -9.59 5.14 -2 0 16 -5.72 6.32 1 0 -16 6.66 5.4 1 0 -16 0.23 4.16 -1 0 16 -13.5 5.74 0 0 -16 -7.73 4.25 0 0 -16 -1.74 5.63 0 0 16 -0.88 7.07 -1 0 -16 1.8 5.97 -1 0 -16 -8.4 5.02 1 0 16 -8.04 6.09 9 -1 -16 -6.15 4.74 -9 1 16 -2.65 8.28 -9 1 16 -11.76 6.67 8 -1 -16 4.17 4.75 -8 1 16 -1.55 8.21 -8 1 16 -3.53 6.7 7 -1 -16 3.07 4.58 -7 1 16 -2.65 8.81 -7 1 16 13.06 6.93 -6 1 16 9.24 6.72 -6 1 16 9.57 9.11 5 -1 -16 11.53 4.1 -5 1 16 10.97 6.68 -5 1 16 11.59 7.75 4 -1 -16 -0.93 3.63 -4 1 16 -0.06 6.26 -4 1 16 -2.09 5.84 3 -1 -16 8.88 4.38 -3 1 16 8.81 6.51 -3 1 16 0.9 6.08 2 -1 -16 -0.88 4.15 2 -1 -16 6.93 5.05 -2 1 16 3.11 5.98 1 -1 -16 -10.12 5.1 1 -1 -16 2.42 4.68 -1 1 16 -3.85 5.99 0 -1 -16 -8.62 5.32 0 -1 -16 -0.93 5.07 0 1 16 0.27 6.53 9 -2 -16 -10.72 4.42 -9 2 16 1.71 7.04 -9 2 16 -7.02 9.7 8 -2 -16 -3.73 4.25 -8 2 16 5.53 10 -8 2 16 3.22 6.52 7 -2 -16 4.71 4.25 -7 2 16 0.98 6.56 -7 2 16 13.46 9.92 6 -2 -16 1.89 3.81 -6 2 16 19.31 7.26 -6 2 16 -5.47 10.04 5 -2 -16 2.73 3.92 -5 2 16 9.34 9.32 -5 2 16 -7.33 5.62 4 -2 -16 2.86 4 -4 2 16 11.37 8.95 -4 2 16 3.25 6.27 -4 2 16 2.52 6.83 3 -2 -16 0.73 3.88 -3 2 16 -8.03 5.64 -3 2 16 8.57 6.68 2 -2 -16 -9.25 5.51 2 -2 -16 3.29 4.56 -2 2 16 -3.53 6.73 -2 2 16 3.83 6.29 1 -2 -16 4.36 5.37 1 -2 -16 -1.96 4.56 -1 2 16 5.4 7.19 -1 2 16 -0.33 6.39 0 -2 -16 -3.81 5.54 0 -2 -16 -0.79 4.98 0 2 16 -5.34 7.24 0 2 16 -1.46 6.72 -9 3 16 3.96 10.72 -9 3 16 -1.88 7.28 8 -3 -16 -9.91 6.98 8 -3 -16 -1.67 4.28 -8 3 16 2.62 5.94 -8 3 16 -5.38 9.66 -8 3 16 -5.02 6.87 7 -3 -16 -9.03 7.03 7 -3 -16 -4.83 3.45 -7 3 16 3.09 6.74 -7 3 16 -0.54 5.57 -7 3 16 -4.71 9.1 6 -3 -16 1.8 4.53 6 -3 -16 0.23 7.29 -6 3 16 3.1 5.61 -6 3 16 1.51 9.49 -6 3 16 -4.37 6.14 5 -3 -16 -0.48 4.04 -5 3 16 -0.71 5.36 -5 3 16 3.26 6.16 4 -3 -16 2.92 4.14 -4 3 16 -5.34 5.57 -4 3 16 -0.57 7.04 3 -3 -16 0.16 4.11 -3 3 16 -4.38 5.7 -3 3 16 1.08 5.57 2 -3 -16 -5.55 3.78 -2 3 16 -5.84 6 -2 3 16 -3.79 5.84 1 -3 -16 -10.81 5.69 1 -3 -16 -2.71 4.38 -1 3 16 -5.59 6.82 -1 3 16 0.03 5.96 8 -4 -16 -5.63 7.89 8 -4 -16 -2.66 5.05 -8 4 16 3.32 6.38 -8 4 16 -6.22 9.7 -8 4 16 -10.64 6.44 7 -4 -16 3.78 4.77 7 -4 -16 -2.64 8.04 -7 4 16 4.19 6.46 -7 4 16 -4.19 5.96 -7 4 16 0.93 10.12 6 -4 -16 -0.66 4.4 6 -4 -16 -15.02 7.43 -6 4 16 6.63 6.54 -6 4 16 0.28 5.85 5 -4 -16 5.32 4.3 -5 4 16 15.57 6.55 -5 4 16 7.84 6.88 4 -4 -16 0.83 3.97 -4 4 16 2.69 6.98 -4 4 16 -8.7 5.78 3 -4 -16 3.5 4.48 -3 4 16 -6.1 6.34 -3 4 16 -7.44 6.19 2 -4 -16 0.61 4.51 -2 4 16 1.46 6.46 -2 4 16 3 6.36 7 -5 -16 1.61 4.75 7 -5 -16 -1.42 7.77 -7 5 16 -4.71 5.95 -7 5 16 -9.96 5.99 6 -5 -16 0.03 7.44 6 -5 -16 -0.12 4.63 -6 5 16 -9.53 5.84 -6 5 16 5.26 6.87 5 -5 -16 -0.44 4.59 -5 5 16 -13.2 6.1 -5 5 16 -5.05 6.94 4 -5 -16 -1.98 4.44 -4 5 16 5.75 6.18 -4 5 16 -4.68 6.24 3 -5 -16 8.18 4.21 -3 5 16 -4.42 6.96 -3 5 16 2.47 8.02 5 5 -17 -1.52 4.52 -5 -5 17 3.19 7.36 4 5 -17 -1.35 4.54 -4 -5 17 -3.98 6.54 -4 -5 17 -12.44 6.8 3 5 -17 -4.94 6.47 3 5 -17 7.12 5.02 -3 -5 17 -4.5 8.49 -3 -5 17 -7.37 6.18 2 5 -17 0.7 5.95 2 5 -17 -2.65 4.54 -2 -5 17 -6.22 6.96 -2 -5 17 -13.39 7.01 6 4 -17 -2.54 4.34 -6 -4 17 1.84 6.87 5 4 -17 -3.73 4.25 -5 -4 17 -12.84 6.13 -5 -4 17 0.95 7.76 4 4 -17 7.24 4.49 -4 -4 17 0.52 6.5 -4 -4 17 -3.33 7.62 3 4 -17 4.2 5.98 3 4 -17 -2.06 3.88 -3 -4 17 -5.35 6.71 -3 -4 17 -10.23 7.24 2 4 -17 5.33 4.57 2 4 -17 3.81 6.41 -2 -4 17 -12.03 6.16 -2 -4 17 -4.81 7.38 1 4 -17 2.33 5.28 1 4 -17 -0.22 6.38 -1 -4 17 -1.06 6.48 -1 -4 17 0.04 8.05 7 3 -17 6.55 5.38 -7 -3 17 2.16 7.31 -7 -3 17 2.18 6.99 6 3 -17 -1.15 4.34 -6 -3 17 5.3 7.27 -6 -3 17 -11.29 5.99 5 3 -17 0.33 4.29 -5 -3 17 -13.8 6.51 -5 -3 17 -8.83 6.36 4 3 -17 4.48 3.92 -4 -3 17 -1.81 6.24 -4 -3 17 -14.73 6.57 3 3 -17 -0.15 4.56 3 3 -17 -8.08 6.29 -3 -3 17 -4.43 5.93 -3 -3 17 -3.47 7.35 2 3 -17 1.95 5.95 2 3 -17 8.7 5.18 -2 -3 17 1.16 6.93 -2 -3 17 -4.32 7.33 1 3 -17 -10.6 5.68 1 3 -17 -3.82 5.35 -1 -3 17 -2.52 7.37 -1 -3 17 -5.04 6.67 7 2 -17 2.42 4.94 -7 -2 17 3.71 8.23 -7 -2 17 -3.78 6.5 6 2 -17 3.71 4.55 -6 -2 17 3.71 6.9 -6 -2 17 -11.04 7.02 5 2 -17 -1.59 4.26 -5 -2 17 -0.7 6.84 -5 -2 17 -4.02 5.86 4 2 -17 -0.57 3.92 -4 -2 17 6.83 7.99 -4 -2 17 -8.28 6.16 3 2 -17 11.2 5.14 -3 -2 17 -3.18 6.09 -3 -2 17 -13.04 6.33 2 2 -17 -6.95 5.52 2 2 -17 -3.19 4.34 -2 -2 17 -11.59 7.01 -2 -2 17 -12.68 6.18 1 2 -17 4.83 5.6 1 2 -17 -6.64 5.61 -1 -2 17 -14.22 5.84 -1 -2 17 -7.26 7.63 8 1 -17 -3.31 4.85 -8 -1 17 3.32 6.93 7 1 -17 2.09 4.85 -7 -1 17 -11.3 6.29 -7 -1 17 -7.57 8.65 6 1 -17 -4.16 3.99 -6 -1 17 0.6 7.24 -6 -1 17 0.24 6.32 5 1 -17 -1.15 3.72 -5 -1 17 5.15 6.64 -5 -1 17 7.7 7.54 4 1 -17 0.25 4.32 -4 -1 17 0.76 6.44 -4 -1 17 -3.76 5.79 3 1 -17 8.34 4.71 -3 -1 17 -4.09 6.63 -3 -1 17 5.34 6.42 2 1 -17 -0.07 4.25 2 1 -17 4.74 6.03 -2 -1 17 5.02 6.75 -2 -1 17 -12.03 6.89 1 1 -17 1.51 6.11 1 1 -17 0.44 5.29 -1 -1 17 4.21 6.85 8 0 -17 4.45 5.53 -8 0 17 -7.94 7.71 -8 0 17 13.26 8.59 7 0 -17 -3.91 4.3 -7 0 17 4.92 6.77 -7 0 17 -3.43 9.09 6 0 -17 1.78 4.29 -6 0 17 -14.12 9.14 -6 0 17 0.75 6.15 5 0 -17 1.22 4.24 -5 0 17 5.2 7.08 -5 0 17 3.84 7.17 4 0 -17 1.36 4.22 -4 0 17 -0.61 6.21 -4 0 17 -0.26 7.15 3 0 -17 0.49 3.94 -3 0 17 -0.79 5.92 -3 0 17 -8.49 6.17 2 0 -17 2.49 4.58 2 0 -17 -0.39 5.87 -2 0 17 5.63 7.16 1 0 -17 -13.3 5.35 1 0 -17 -0.2 4.7 -1 0 17 -7.87 6.03 8 -1 -17 -4.2 4.77 -8 1 17 5.03 7.33 7 -1 -17 -6.24 3.71 -7 1 17 -10.36 9.54 -7 1 17 -3.9 6.86 6 -1 -17 7.24 4.39 -6 1 17 9.12 6.6 -6 1 17 1.35 10.36 5 -1 -17 8.91 4.5 -5 1 17 4.04 6.96 -5 1 17 -0.27 7.22 4 -1 -17 8.43 4.47 -4 1 17 4.87 6.11 -4 1 17 -5.45 6.02 3 -1 -17 -4.91 3.53 -3 1 17 -1.73 6.47 2 -1 -17 -4.08 3.86 -2 1 17 3.33 6.15 7 -2 -17 -0.14 4.68 -7 2 17 -10.14 6.62 -7 2 17 -16.08 9.94 6 -2 -17 -1.47 4.4 -6 2 17 -8.86 6.51 -6 2 17 -10.19 10.89 5 -2 -17 5.37 4.13 -5 2 17 8.31 7.26 4 -2 -17 -2.68 4.08 -4 2 17 -6.31 5.77 3 -2 -17 -0.81 4.3 -3 2 17 4.3 6.48 6 -3 -17 1.78 4.29 -6 3 17 -3.97 6.98 5 -3 -17 4.52 4.96 -5 3 17 -4.09 5.88 4 -3 -17 0.35 4.22 -4 3 17 -2.38 6.87 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N5 100.0(3) . . ? N1 Ni1 N2 78.9(3) . . ? N1 Ni1 O2 91.9(3) . . ? N1 Ni1 O1 86.5(3) . . ? N1 Ni1 N4 179.3(3) . . ? N5 Ni1 N2 88.7(3) . . ? N5 Ni1 O2 90.0(3) . . ? N5 Ni1 O1 173.5(3) . . ? N2 Ni1 O1 92.9(3) . . ? O2 Ni1 N2 170.3(3) . . ? O2 Ni1 O1 89.4(3) . . ? N4 Ni1 N5 79.6(3) . . ? N4 Ni1 N2 100.5(3) . . ? N4 Ni1 O2 88.7(3) . . ? N4 Ni1 O1 93.9(3) . . ? C23 N1 Ni1 116.6(6) . . ? C19 N1 Ni1 126.4(8) . . ? C19 N1 C23 117.0(9) . . ? C6 N5 Ni1 112.1(6) . . ? C12 N5 Ni1 139.3(6) . . ? C12 N5 C6 107.6(8) . . ? C24 N2 Ni1 113.1(6) . . ? C30 N2 Ni1 139.0(6) . . ? C30 N2 C24 107.2(8) . . ? Ni1 O2 H2A 96(7) . . ? Ni1 O2 H2B 95(7) . . ? H2A O2 H2B 102(5) . . ? Ni1 O1 H1A 104.0 . . ? Ni1 O1 H1B 103.8 . . ? H1A O1 H1B 104.5 . . ? C5 N4 Ni1 115.8(6) . . ? C5 N4 C1 119.4(10) . . ? C1 N4 Ni1 124.8(8) . . ? C30 N3 C25 109.0(8) . . ? C30 N3 C29 127.6(9) . . ? C29 N3 C25 123.3(9) . . ? C12 N6 C7 109.5(8) . . ? C12 N6 C11 128.0(10) . . ? C11 N6 C7 122.6(9) . . ? N1 C23 C24 112.9(8) . . ? N1 C23 C22 120.6(9) . . ? C22 C23 C24 126.4(10) . . ? N2 C24 C23 117.9(8) . . ? C25 C24 N2 112.1(8) . . ? C25 C24 C23 129.9(9) . . ? N3 C25 C26 115.3(9) . . ? C24 C25 N3 103.3(8) . . ? C24 C25 C26 141.3(10) . . ? N2 C30 N3 108.3(8) . . ? N2 C30 C31 128.3(11) . . ? N2 C30 C38 124(2) . . ? N3 C30 C31 122.3(11) . . ? N3 C30 C38 127(2) . . ? N5 C6 C5 118.0(8) . . ? N5 C6 C7 109.5(9) . . ? C7 C6 C5 132.5(9) . . ? N5 C12 C13 127.3(9) . . ? N6 C12 N5 109.1(9) . . ? N6 C12 C13 123.5(9) . . ? C23 C22 H22 121.5 . . ? C23 C22 C21 116.9(12) . . ? C21 C22 H22 121.5 . . ? N4 C5 C6 113.9(8) . . ? N4 C5 C4 123.4(10) . . ? C4 C5 C6 122.6(10) . . ? C12 C13 C18 113.5(10) . . ? C12 C13 C18A 113.8(17) . . ? C14 C13 C12 128.7(11) . . ? C14 C13 C18 117.9(13) . . ? C14A C13 C12 130.0(16) . . ? C14A C13 C18A 116(2) . . ? C32 C31 C30 114.7(13) . . ? C36 C31 C30 126.6(17) . . ? C36 C31 C32 118.7(16) . . ? C6 C7 N6 104.3(8) . . ? C6 C7 C8 135.9(11) . . ? C8 C7 N6 119.7(10) . . ? C25 C26 H26 119.0 . . ? C27 C26 C25 122.1(11) . . ? C27 C26 H26 119.0 . . ? C5 C4 H4 122.5 . . ? C5 C4 C3 114.9(11) . . ? C3 C4 H4 122.5 . . ? N6 C11 H11 121.4 . . ? N6 C11 C10 117.1(12) . . ? C10 C11 H11 121.4 . . ? N1 C19 H19 117.8 . . ? N1 C19 C20 124.3(13) . . ? C20 C19 H19 117.8 . . ? C26 C27 H27 120.3 . . ? C26 C27 C28 119.5(11) . . ? C28 C27 H27 120.3 . . ? N4 C1 H1 120.5 . . ? N4 C1 C2 119.0(13) . . ? C2 C1 H1 120.5 . . ? C27 C28 H28 119.9 . . ? C29 C28 C27 120.3(11) . . ? C29 C28 H28 119.9 . . ? C7 C8 H8 121.7 . . ? C9 C8 C7 116.6(12) . . ? C9 C8 H8 121.7 . . ? C4 C3 H3 118.7 . . ? C2 C3 C4 122.6(12) . . ? C2 C3 H3 118.7 . . ? C31 C32 H32 120.5 . . ? C33 C32 C31 119.0(17) . . ? C33 C32 H32 120.5 . . ? C22 C21 H21 119.9 . . ? C20 C21 C22 120.3(12) . . ? C20 C21 H21 119.9 . . ? N3 C29 H29 120.3 . . ? C28 C29 N3 119.4(11) . . ? C28 C29 H29 120.3 . . ? C19 C20 H20 119.6 . . ? C21 C20 C19 120.7(13) . . ? C21 C20 H20 119.6 . . ? C13 C18 H18 122.8 . . ? C17 C18 C13 114.3(12) . . ? C17 C18 H18 122.8 . . ? C13 C14 Br2 118.2(12) . . ? C13 C14 C15 124.6(14) . . ? C15 C14 Br2 117.2(11) . . ? C1 C2 H2 119.7 . . ? C3 C2 C1 120.6(14) . . ? C3 C2 H2 119.7 . . ? C11 C10 H10 119.5 . . ? C11 C10 C9 120.9(12) . . ? C9 C10 H10 119.5 . . ? C8 C9 C10 123.1(12) . . ? C8 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C14 C15 H15 122.7 . . ? C16 C15 C14 114.5(16) . . ? C16 C15 H15 122.7 . . ? C33 C34 H34 115.5 . . ? C35 C34 H34 115.5 . . ? C35 C34 C33 129.1(19) . . ? C32 C33 C34 114.4(17) . . ? C32 C33 H33 122.8 . . ? C34 C33 H33 122.8 . . ? C15 C16 H16 115.9 . . ? C15 C16 C17 128.1(17) . . ? C17 C16 H16 115.9 . . ? C34 C35 H35 122.7 . . ? C34 C35 C36 114.7(19) . . ? C36 C35 H35 122.7 . . ? C18 C17 H17 120.0 . . ? C16 C17 C18 119.9(15) . . ? C16 C17 H17 120.0 . . ? C31 C36 Br1 121.8(13) . . ? C31 C36 C35 124(2) . . ? C35 C36 Br1 114.0(14) . . ? C37 C2A Br4 114(2) . . ? C38 C2A Br4 118.3(18) . . ? C38 C2A C37 125(3) . . ? C2A C37 H37 122.8 . . ? C40 C37 C2A 114(3) . . ? C40 C37 H37 122.8 . . ? C2A C38 C30 118(2) . . ? C2A C38 C0 119(2) . . ? C0 C38 C30 122(2) . . ? C38 C0 H0 121.6 . . ? C39 C0 C38 117(2) . . ? C39 C0 H0 121.6 . . ? C0 C39 H39 122.7 . . ? C0 C39 C40 115(2) . . ? C40 C39 H39 122.7 . . ? C37 C40 C39 127(3) . . ? C37 C40 H40 116.3 . . ? C39 C40 H40 116.3 . . ? H3A O3 H3B 102(5) . . ? C13 C18A H18A 122.7 . . ? C17A C18A C13 115(2) . . ? C17A C18A H18A 122.7 . . ? C13 C14A C15A 127(2) . . ? C13 C14A Br2A 108.3(18) . . ? C15A C14A Br2A 120(2) . . ? C14A C15A H15A 123.3 . . ? C16A C15A C14A 113(3) . . ? C16A C15A H15A 123.3 . . ? C15A C16A H16A 115.9 . . ? C15A C16A C17A 128(3) . . ? C17A C16A H16A 115.9 . . ? C18A C17A H17A 119.8 . . ? C16A C17A C18A 120(3) . . ? C16A C17A H17A 119.8 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.071(7) . ? Ni1 N5 2.085(7) . ? Ni1 N2 2.108(7) . ? Ni1 O2 2.095(7) . ? Ni1 O1 2.124(7) . ? Ni1 N4 2.075(8) . ? Br1 C36 1.87(2) . ? Br2 C14 1.898(15) . ? N1 C23 1.380(13) . ? N1 C19 1.333(11) . ? N5 C6 1.376(11) . ? N5 C12 1.352(12) . ? N2 C24 1.363(10) . ? N2 C30 1.344(11) . ? O2 H2A 0.85(2) . ? O2 H2B 0.86(2) . ? O1 H1A 0.8496 . ? O1 H1B 0.8497 . ? N4 C5 1.350(12) . ? N4 C1 1.359(13) . ? N3 C25 1.428(12) . ? N3 C30 1.355(12) . ? N3 C29 1.390(13) . ? N6 C12 1.332(11) . ? N6 C7 1.416(13) . ? N6 C11 1.362(12) . ? C23 C24 1.475(12) . ? C23 C22 1.396(13) . ? C24 C25 1.341(13) . ? C25 C26 1.430(14) . ? C30 C31 1.472(17) . ? C30 C38 1.46(2) . ? C6 C5 1.468(14) . ? C6 C7 1.376(13) . ? Cl3 Cl3 2.33(4) 2_576 ? C12 C13 1.485(16) . ? C22 H22 0.9300 . ? C22 C21 1.436(17) . ? C5 C4 1.370(13) . ? C13 C18 1.563(18) . ? C13 C14 1.286(19) . ? C13 C18A 1.59(2) . ? C13 C14A 1.26(3) . ? C31 C32 1.46(2) . ? C31 C36 1.35(2) . ? C7 C8 1.392(13) . ? C26 H26 0.9300 . ? C26 C27 1.340(16) . ? C4 H4 0.9300 . ? C4 C3 1.431(17) . ? C11 H11 0.9300 . ? C11 C10 1.376(16) . ? C19 H19 0.9300 . ? C19 C20 1.344(16) . ? C27 H27 0.9300 . ? C27 C28 1.477(16) . ? C1 H1 0.9300 . ? C1 C2 1.406(17) . ? C28 H28 0.9300 . ? C28 C29 1.329(15) . ? C8 H8 0.9300 . ? C8 C9 1.373(17) . ? C3 H3 0.9300 . ? C3 C2 1.285(18) . ? C32 H32 0.9300 . ? C32 C33 1.39(2) . ? C21 H21 0.9300 . ? C21 C20 1.286(19) . ? C29 H29 0.9300 . ? C20 H20 0.9300 . ? C18 H18 0.9300 . ? C18 C17 1.41(2) . ? C14 C15 1.49(2) . ? C2 H2 0.9300 . ? C10 H10 0.9300 . ? C10 C9 1.383(19) . ? C9 H9 0.9300 . ? C15 H15 0.9300 . ? C15 C16 1.27(2) . ? C34 H34 0.9300 . ? C34 C33 1.440(16) . ? C34 C35 1.28(3) . ? C33 H33 0.9300 . ? C16 H16 0.9300 . ? C16 C17 1.367(14) . ? C35 H35 0.9300 . ? C35 C36 1.396(19) . ? C17 H17 0.9300 . ? Br4 C2A 1.85(2) . ? C2A C37 1.36(2) . ? C2A C38 1.34(2) . ? C37 H37 0.9300 . ? C37 C40 1.26(3) . ? C38 C0 1.45(2) . ? C0 H0 0.9300 . ? C0 C39 1.40(3) . ? C39 H39 0.9300 . ? C39 C40 1.49(2) . ? C40 H40 0.9300 . ? O3 H3A 0.85(2) . ? O3 H3B 0.86(2) . ? C18A H18A 0.9300 . ? C18A C17A 1.40(3) . ? C14A C15A 1.49(3) . ? C14A Br2A 1.89(2) . ? C15A H15A 0.9300 . ? C15A C16A 1.27(3) . ? C16A H16A 0.9300 . ? C16A C17A 1.36(2) . ? C17A H17A 0.9300 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni1 N1 C23 C24 0.6(9) . . . . ? Ni1 N1 C23 C22 179.1(6) . . . . ? Ni1 N1 C19 C20 177.8(8) . . . . ? Ni1 N5 C6 C5 7.1(9) . . . . ? Ni1 N5 C6 C7 -171.6(6) . . . . ? Ni1 N5 C12 N6 168.2(6) . . . . ? Ni1 N5 C12 C13 -8.9(14) . . . . ? Ni1 N2 C24 C23 8.8(9) . . . . ? Ni1 N2 C24 C25 -173.4(6) . . . . ? Ni1 N2 C30 N3 169.5(7) . . . . ? Ni1 N2 C30 C31 1.6(18) . . . . ? Ni1 N2 C30 C38 -21(2) . . . . ? Ni1 N4 C5 C6 -2.1(9) . . . . ? Ni1 N4 C5 C4 179.5(7) . . . . ? Ni1 N4 C1 C2 -179.6(8) . . . . ? Br2 C14 C15 C16 -178.3(14) . . . . ? N1 C23 C24 N2 -6.4(10) . . . . ? N1 C23 C24 C25 176.3(9) . . . . ? N1 C23 C22 C21 3.2(13) . . . . ? N1 C19 C20 C21 2.5(19) . . . . ? N5 C6 C5 N4 -3.5(11) . . . . ? N5 C6 C5 C4 174.9(8) . . . . ? N5 C6 C7 N6 0.0(9) . . . . ? N5 C6 C7 C8 -179.3(11) . . . . ? N5 C12 C13 C18 -71.9(14) . . . . ? N5 C12 C13 C14 109.3(18) . . . . ? N5 C12 C13 C18A 105(3) . . . . ? N5 C12 C13 C14A -66(4) . . . . ? N2 C24 C25 N3 1.3(10) . . . . ? N2 C24 C25 C26 179.0(11) . . . . ? N2 C30 C31 C32 -78.9(18) . . . . ? N2 C30 C31 C36 102(2) . . . . ? N2 C30 C38 C2A 110(3) . . . . ? N2 C30 C38 C0 -57(4) . . . . ? N4 C5 C4 C3 -0.4(14) . . . . ? N4 C1 C2 C3 0.8(18) . . . . ? N3 C25 C26 C27 -2.8(13) . . . . ? N3 C30 C31 C32 114.7(15) . . . . ? N3 C30 C31 C36 -64(2) . . . . ? N3 C30 C38 C2A -83(4) . . . . ? N3 C30 C38 C0 111(4) . . . . ? N6 C12 C13 C18 111.5(12) . . . . ? N6 C12 C13 C14 -67.3(19) . . . . ? N6 C12 C13 C18A -72(3) . . . . ? N6 C12 C13 C14A 117(3) . . . . ? N6 C7 C8 C9 0.4(14) . . . . ? N6 C11 C10 C9 -0.1(17) . . . . ? C23 N1 C19 C20 0.8(14) . . . . ? C23 C24 C25 N3 178.7(8) . . . . ? C23 C24 C25 C26 -3.6(19) . . . . ? C23 C22 C21 C20 0.1(17) . . . . ? C24 N2 C30 N3 0.2(10) . . . . ? C24 N2 C30 C31 -167.8(12) . . . . ? C24 N2 C30 C38 169.4(16) . . . . ? C24 C23 C22 C21 -178.5(9) . . . . ? C24 C25 C26 C27 179.7(11) . . . . ? C25 N3 C30 N2 0.6(11) . . . . ? C25 N3 C30 C31 169.4(11) . . . . ? C25 N3 C30 C38 -168.2(15) . . . . ? C25 N3 C29 C28 -2.0(16) . . . . ? C25 C26 C27 C28 -0.3(16) . . . . ? C30 N2 C24 C23 -178.7(8) . . . . ? C30 N2 C24 C25 -1.0(10) . . . . ? C30 N3 C25 C24 -1.2(10) . . . . ? C30 N3 C25 C26 -179.5(8) . . . . ? C30 N3 C29 C28 -177.7(10) . . . . ? C30 C31 C32 C33 177.0(14) . . . . ? C30 C31 C36 Br1 -1(3) . . . . ? C30 C31 C36 C35 -174.8(17) . . . . ? C30 C38 C0 C39 -179(3) . . . . ? C6 N5 C12 N6 1.2(9) . . . . ? C6 N5 C12 C13 -175.8(8) . . . . ? C6 C5 C4 C3 -178.7(8) . . . . ? C6 C7 C8 C9 179.6(11) . . . . ? C12 N5 C6 C5 178.0(7) . . . . ? C12 N5 C6 C7 -0.7(9) . . . . ? C12 N6 C7 C6 0.7(9) . . . . ? C12 N6 C7 C8 -179.8(9) . . . . ? C12 N6 C11 C10 179.5(10) . . . . ? C12 C13 C18 C17 174.1(13) . . . . ? C12 C13 C14 Br2 0(2) . . . . ? C12 C13 C14 C15 -179.3(14) . . . . ? C12 C13 C18A C17A -178(4) . . . . ? C12 C13 C14A C15A -178(4) . . . . ? C12 C13 C14A Br2A -23(5) . . . . ? C22 C23 C24 N2 175.2(8) . . . . ? C22 C23 C24 C25 -2.1(14) . . . . ? C22 C21 C20 C19 -3(2) . . . . ? C5 N4 C1 C2 0.2(14) . . . . ? C5 C6 C7 N6 -178.5(9) . . . . ? C5 C6 C7 C8 2.2(19) . . . . ? C5 C4 C3 C2 1.5(17) . . . . ? C13 C18 C17 C16 9(2) . . . . ? C13 C14 C15 C16 1(3) . . . . ? C13 C18A C17A C16A 1(8) . . . . ? C13 C14A C15A C16A -11(8) . . . . ? C31 C32 C33 C34 1.2(15) . . . . ? C7 N6 C12 N5 -1.2(10) . . . . ? C7 N6 C12 C13 175.9(8) . . . . ? C7 N6 C11 C10 0.3(14) . . . . ? C7 C6 C5 N4 174.9(9) . . . . ? C7 C6 C5 C4 -6.7(15) . . . . ? C7 C8 C9 C10 -0.2(17) . . . . ? C26 C27 C28 C29 2.6(17) . . . . ? C4 C3 C2 C1 -2(2) . . . . ? C11 N6 C12 N5 179.5(9) . . . . ? C11 N6 C12 C13 -3.3(14) . . . . ? C11 N6 C7 C6 -179.9(8) . . . . ? C11 N6 C7 C8 -0.5(13) . . . . ? C11 C10 C9 C8 0.0(19) . . . . ? C19 N1 C23 C24 177.8(7) . . . . ? C19 N1 C23 C22 -3.6(12) . . . . ? C27 C28 C29 N3 -1.4(18) . . . . ? C1 N4 C5 C6 178.0(8) . . . . ? C1 N4 C5 C4 -0.3(13) . . . . ? C32 C31 C36 Br1 -179.8(13) . . . . ? C32 C31 C36 C35 6(3) . . . . ? C29 N3 C25 C24 -177.5(9) . . . . ? C29 N3 C25 C26 4.1(13) . . . . ? C29 N3 C30 N2 176.8(9) . . . . ? C29 N3 C30 C31 -14.4(18) . . . . ? C29 N3 C30 C38 8(2) . . . . ? C18 C13 C14 Br2 -178.8(11) . . . . ? C18 C13 C14 C15 2(3) . . . . ? C14 C13 C18 C17 -7(2) . . . . ? C14 C15 C16 C17 2(3) . . . . ? C15 C16 C17 C18 -7(3) . . . . ? C34 C35 C36 Br1 -179.9(12) . . . . ? C34 C35 C36 C31 -5(3) . . . . ? C33 C34 C35 C36 3(2) . . . . ? C35 C34 C33 C32 -0.7(17) . . . . ? C36 C31 C32 C33 -4(2) . . . . ? Br4 C2A C37 C40 180(3) . . . . ? Br4 C2A C38 C30 12(5) . . . . ? Br4 C2A C38 C0 179(3) . . . . ? C2A C37 C40 C39 -11(6) . . . . ? C2A C38 C0 C39 14(6) . . . . ? C37 C2A C38 C30 172(4) . . . . ? C37 C2A C38 C0 -22(7) . . . . ? C38 C2A C37 C40 20(6) . . . . ? C38 C0 C39 C40 -7(5) . . . . ? C0 C39 C40 C37 6(6) . . . . ? C18A C13 C14A C15A 11(7) . . . . ? C18A C13 C14A Br2A 167(3) . . . . ? C14A C13 C18A C17A -6(6) . . . . ? C14A C15A C16A C17A 4(9) . . . . ? C15A C16A C17A C18A -1(9) . . . . ? Br2A C14A C15A C16A -164(4) . . . . ?